Fagus sylvatica) and isolated from diseased trees and healthy trees were examined in relation to their impact on tree health. To this end, classical culture-based isolation methods, in planta inoculations and fungal identification using ITS-barcode and morphological characters were used. Stem endophytes of healthy beech saplings collected in German forests were isolated to determine endophyte communities in woody stem tissues. Pathogenicity tests were performed on living potted beech saplings using twelve selected fungal pathogens and wood inhabiting fungi  originating mainly from European beech with symptoms of the complex disease Vitality loss, or from bark necroses, or known to be common endophytes of beech. The impact of these ascomycetous fungi with respect to tree health was discussed. The potential influences of endophytic fungi of beech and of test conditions are discussed in relation to the success of inoculation. All tested fungal strains except for Neonectria ditissima were able to establish themselves post inoculation in the beech stems and caused necroses when there was sufficient water, but at different severities. Under the experimental conditions, Botryosphaeria corticola was shown to be the most virulent tested latent pathogen against F. sylvatica. In the context of climate change and global warming, the tested Botryosphaeriaceae are able to play a primary role in the disease progress of Vitality loss of Beech. The key role of Neonectria coccinea in causing bark necroses and the loss of vitality in beech was confirmed because the tested strain induced large lesions on the beech saplings.Filamentous fungi associated with woody tissues of European Beech ( Fagus sylvatica L.) is one of the major tree species in Central Europe and has an important impact on the ecology and hydrogeology of forests  relative to the reference period 1961–1990. In the year of our study, 2020, the total precipitation across Germany was 710 l/m2 (a deficit of -10%) and in Lower Saxony it was only 689 l/m2 (a deficit of -13%). Generally, periods of soil moisture drought stress can last longer than the meteorological drought that causes them and can have negative effects on plants or tree growth and health  S. Hughes, Apiognomonia errabunda (Roberge ex Desm.) Höhn., Biscogniauxia nummularia (Bull.) Kuntze, Hypoxylon fragiforme (Pers.) J. Kickx f., and Neonectria coccinea (Pers.) Rossman and Samuels , were found for the first time to be associated with the woody tissues of beech, or represented the first discovery on beech in Germany [Sphaeropsis sapinea (Fr.) Dyko and B. Sutton]  to confirm the pathogenicity and virulence in planta of latent fungal pathogens originally associated with bark necrosis or VLB, (2) to test virulence of the fungal species under field conditions in vital trees not exposed to drought stress, and (3) to determine whether there are interactions between beech stem endophytes and the inoculated pathogens. Therefore, the virulence of these endophytes in relation to the production of bark necroses and as potential pathogens of European beech was tested in inoculation tests involving potted beech saplings growing under field conditions.Acer pseudoplatanus L. and Fagus sylvatica L.) sampled in Germany  and the stem diameter 70 cm above ground was 0.96 – 2.05 cm . The saplings were planted in 65 l black plant pots containing potting compost . The 137 plants were randomly assigned to blocks and kept at natural air temperature . They were watered regularly via a Drip irrigation system  and shaded by surrounding older trees. During the experiment the watering regime was adjusted to supply the saplings with the optimal amount of water and air temperatures were measured by a HOBO® Pro v2 data logger. The endophyte community in the woody tissues of the plant material collected from the natural beech regeneration site was determined prior to the experiment. Three saplings were examined to determine whether there was pre-colonization of the internal tissues by the test species and to profile the endophyte community. After surface disinfection with a 70% ethanol spray, stem bark and small wood chips  were obtained and placed in Petri dishes with culture medium, then incubated at room temperature in daylight. They were cultivated on malt yeast peptone agar (MYP), modified according to The saplings were excavated from a natural regeneration stand in March 2020 . The health of the saplings appeared to be very good at the beginning of the experiment and no symptoms of Vitality loss, bark necrosis or other disease symptoms were visible. The stem height of the saplings was 169 –327 cm  to identify similar ITS sequences. A similarity threshold of 98% was set for species-level identification. Generally, morphological characteristics were used to confirm the results of molecular identification.Following Altschul et al., 1997Neonectria ditissima (CBS 226.31) all fungal strains used in our pathogenicity tests were isolated from material associated with cases of disease from Germany that have been studied by the NW-FVA. Apart from Nectria cinnabarina  all tested strains were isolated from woody tissues or bark necrotic tissue of diseased European beech trees following the procedure described above for endophytes from fruiting bodies growing on these trees. They were identified based on morphology and ITS sequencing. The ITS sequences  have been deposited in GenBank ; B. dothidea (Moug.) Ces. and De Not., anamorph: Fusicoccum aesculi Corda, NW-FVA 5287: Saxony-Anhalt; B. stevensii Shoemaker, anamorph: Diplodia mutila (Fr.) Mont., NW-FVA 4915, Hesse; and Sphaeropsis sapinea, synonym: Diplodia sapinea (Fr.) Fuckel , Diatrypaceae , Graphostromataceae , Hypoxylaceae , and Nectriaceae .With the exception of  GenBank  and all  GenBank  includedN. cinnabarina), ten saplings were inoculated with an MYP-agar plug of a one-week-old culture of the fungus. The plugs were placed in wounds made with a sterile cork borer (5 mm diameter) in the stem at a height of 70 cm. The removed bark was replaced on top of the plug, then the stem was wrapped with Parafilm. A set of 10 untreated controls, trees which were not inoculated at all, and mock controls, prepared by inoculating 10 trees with a sterile pure culture medium plug of MYP, were created. After 4 weeks (29.06.2020) one sapling per treatment group was sampled to check infection success and necrosis formation. The bark around the area of inoculation was peeled away to allow us to see and measure the extent of any necroses. Lesion lengths were measured with a ruler in the vertical direction to an accuracy of 1 mm. Fungi were re-isolated from discolored and non-discolored tissue and the resulting isolates were identified. The pathogenicity tests ended four months after inoculation with the twelve potential latent pathogens. The impact on tree health of each strain was estimated on the basis of the size of the necrotic lesions. In addition, the reaction of the host tissue, such as healing over, formation of a callus, or T-shaped discolorations, was recorded. The latter are dark or black colored T-shaped defects/discoloration of the wood, visible in a cross-section of the stem, caused by healing over of a wound or bark necrosis. Statistical differences in length of the necrotic area between different strains and controls were investigated using ANOVA and Tukey’s HSD post hoc test. All data analysis was conducted in R, version 3.6.2  Fr., Jackrogersella cohaerens (Pers.) L. Wendt, Kuhnert and M. Stadler, Lepteutypa fuckelii Petr., Nigrospora oryzae (Berk. and Broome) Petch, and Penicillium glandicola (Oudem.) Seifert and Samson. All the species that were shown to be present as endophytes, with the exception of the white-rot fungus Coprinellus micaceus (Bull.) Vilgalys, Hopple and Jacq. Johnson, Agaricaceae Basidiomycota, were members of the Ascomycota. Only one of the test species for the inoculation tests, H. fragiforme, was isolated as an endophyte from beech stems.In total, we were able to isolate 18 filamentous, endophytic fungal species from the 89 inocula retrieved from stem bark and wood of the three beech saplings sampled at the beginning of the study . Three sNeonectria ditissima, all the species used for inoculation could be isolated from the inoculated saplings four months after treatment  were isolated from the saplings inoculated with Neo. ditissima. As well as Fusarium sp. and Diaporthe sp., the same Clitopilus sp. was isolated from the saplings inoculated with S. sapinea.Four weeks post inoculation, necrosis formation was not obvious in any of the trees inoculated with the test strains. In untreated and mock controls no necrotic lesions were visible and no fungi could be isolated from the beech tissue in the area of inoculation. Apart from reatment . In addireatment . Three d2 (−59% compared to the mean) in May, 16.6°C (−8% compared to the mean) in June, 65 l/m2 (−11% compared to the mean) in July, 65 l/m2 (−7.1% compared to the mean) in August, and 45 l/m2 (25% of the mean) in September.The months during which the field experiment took place were significantly warmer in Germany than the long-term mean for the international reference period 1961–1990 . The mean air temperature of Lower Saxony was 16.6°C (+ 2.1 compared to the mean) in June, 17.5°C (−0.1°compared to the mean) in July, 20.1°C (+ 3.6°compared to the mean) in August, and 14.5°C (+ 1°compared to the mean) in September. During the pathogenicity tests the mean air temperature was 17°C and 42 days with air temperatures over 25°C, including 8 days ≥ 30°C were recorded at Hann. Münden. The total mean precipitation in Lower Saxony was 25 l/mB. corticola exhibited the largest necrotic areas, and these were significantly larger than all other lesions , followed by saplings inoculated with E. quaternata (19.3 mm), Neo. coccinea (17.9 mm), Neo. aff. coccinea (16.4 mm), Bi. nummularia (13.9 mm), Bo. stevensii (12.8 mm), Bo. dothidea (11.6 mm), Bi. mediterranea (11.3 mm), Neo. ditissima (10.7 mm), S. sapinea (10.7 mm), and H. fragiforme (10.4 mm). Occlusion of the wounds caused by the cork borer was observed in some or all treated saplings inoculated with Bi. mediterranea, Bo. dothidea, Bo. stevensii, H. fragiforme, Neo. ditissima, and S. sapinea within four months. As well as for Bo. corticola, no healing over within four months was recorded in the saplings inoculated with Nec. cinnabarina, Neo. coccinea, Neo. aff. coccinea, Bi. nummularia, and E. quaternata. T-shaped discolorations were visible in saplings inoculated with Bo. dothidea, H. fragiforme, Neo. ditissima, and S. sapinea.At the end of the experiment, all saplings were still alive but exhibiting different reactions to the various treatments , 2. In tBi. mediterranea, H. fragiforme, Neo. ditissima, and S. sapinea. This suggests a lower virulence compared to the other test strains. These fungal strains could, at least, be quiescent colonizers functioning as endophytes after the wounds have healed. Our results showing that all of the tested fungal species induced necrosis in the saplings are not surprising because they are known to be latent pathogenic wood-decaying fungi of F. sylvatica or common pathogens of other tree species. Nevertheless, a single stem infection via wounding and inoculation of a beech sapling with the test species was not sufficient to kill the whole the tree within the four months of the experiment. With the exception of Neo. ditissima, all test strains could be re-isolated, indicating successful infection by these strains and establishment in the woody tissue. In the following, the fungi examined are discussed mainly in the order of induced necrosis length.With the exception of the mock-controls, all inoculations with fungal mycelium via wounding led to the presence of necrotic lesions. In some cases wounds with fungal inoculation were able to heal completely or nearly so within four months; the species for which this happened included Bo. corticola, which differs from the other tested Botryosphaeriaceae in its virulence with regard to F. sylvatica. Bo. corticola is a latent plant pathogen which has been isolated at high frequency from physiologically impaired trees  was smaller than those caused by Bo. stevensii (mean: 73.1 mm), while branches inoculated with S. sapinea showed no visible lesions. The results of our study suggest that with an adequate water supply and the mean air temperature of 17°C maintained during the experiment, B. corticola is significantly more virulent as a wound pathogen than Bo. stevensii. The inoculation experiments in planta showed, that Bo. corticola can be a highly virulent wound pathogen of European beech. If it should turn out that Bo. corticola is a frequent endophyte of European beech, there is an increased risk in the context of climate change or global warming, since it is a weak pathogen with optimal growth in vitro at 25°C  Castl. and Rossman occurring on beech in Europe. The tested strain, NW-FVA 0179, was intermediate between the two latter species with respect to its ITS region. For further studies, we consider that it will be crucial to determine the Neo. aff. coccinea involved more precisely using the methods of Neo. coccinea group have a high capacity to cause necrosis and may lead to tree mortality. Under conditions associated with global warming, increased damage caused by Neo. coccinea is to be expected, since strains of this species exhibit robust, rapid mycelial growth at 30°C in vitro  because the species is able to overgrow necrotic tissues induced by other fungi  and the temperature (negative correlation) – have a significant influence on the dispersal of Bi. mediterranea spores, host tissue colonization and disease outbreaks, necrosis formation seems to be promoted by water stress in the host tree  in clusters on the bark of dead beech or dead areas on living trees. The results of our pathogenicity tests confirm those reported by H. fragiforme is able to form necrotic lesions on beech. The lesions induced by H. fragiforme were significantly smaller during our experiment under elevated temperatures than caused by Bi. nummularia. This fits the results of H. fragiforme decreased at temperatures between 25 and 30°C. H. fragiforme appeared to be less virulent against beech than the other Xylariales species and co-occurred with Neo. coccinea.The wood-decaying species  tissues  but also tissues . The traactivity . Next toof beech , occurriof beech . UsuallyNeo. coccinea, Bi. nummularia, Bo. corticola, Bo. dothidea, Bo. stevensii, and E. quaternata, are sensitive to changes in host physiology driven by stress conditions, as predicted by Latent plant pathogenic fungi of beech that exhibit endophytic behavior, such as Neo. coccinea, Bi. nummularia and plant pathogens, such as Bo. corticola, Nec. cinnabarina, or E. quaternata. Latency units, mainly of Neo. coccinea, appeared to be activated by the host stressors wounding and/or inoculation with fungal species. The observations made in our pathogenicity tests do not allow definitive statements regarding the interactions between the co-occurring fungi and the impact on necrosis formation. Because it is not possible to obtain test saplings without endophytes, it is important in the future to carry out co-occurrence studies or antagonist tests in vitro with latent pathogens. In addition, any experiments should be repeated under different temperature conditions and different water availabilities for the host trees.The elevated temperatures during our pathogenicity tests, which are a consequence of the current climate change in Germany, favored establishment and growth of the early-colonizing species, e.g., https://www.ncbi.nlm.nih.gov/genbank/, MT561410; https://www.ncbi.nlm.nih.gov/genbank/, MT561409; https://www.ncbi.nlm.nih.gov/genbank/, MT561409; https://www.ncbi.nlm.nih.gov/genbank/, MN698983; https://www.ncbi.nlm.nih.gov/genbank/, MZ045841; https://www.ncbi.nlm.nih.gov/genbank/, MN698981; https://www.ncbi.nlm.nih.gov/genbank/, MZ045842; https://www.ncbi.nlm.nih.gov/genbank/, MZ045843; https://www.ncbi.nlm.nih.gov/genbank/, MN698988; https://www.ncbi.nlm.nih.gov/genbank/, JF735309; https://www.ncbi.nlm.nih.gov/genbank/, MN698984; https://www.ncbi.nlm.nih.gov/genbank/, MZ045858; https://www.ncbi.nlm.nih.gov/genbank/, MZ045857; https://www.ncbi.nlm.nih.gov/genbank/, MZ045844; https://www.ncbi.nlm.nih.gov/genbank/, MZ045845; https://www.ncbi.nlm.nih.gov/genbank/, MZ045846; https://www.ncbi.nlm.nih.gov/genbank/, MZ045847; https://www.ncbi.nlm.nih.gov/genbank/, MZ045848; https://www.ncbi.nlm.nih.gov/genbank/, MZ045849; https://www.ncbi.nlm.nih.gov/genbank/, MZ045850; https://www.ncbi.nlm.nih.gov/genbank/, MZ045851; https://www.ncbi.nlm.nih.gov/genbank/, MZ045852; https://www.ncbi.nlm.nih.gov/genbank/, MZ045853; https://www.ncbi.nlm.nih.gov/genbank/, MZ045854; https://www.ncbi.nlm.nih.gov/genbank/, MZ045855; https://www.ncbi.nlm.nih.gov/genbank/, MZ045856; https://www.ncbi.nlm.nih.gov/genbank/, MZ045914; https://www.ncbi. nlm.nih.gov/genbank/, MZ573778.The datasets presented in this study can be found in online repositories. The names of the repository/repositories and accession number(s) can be found below: JB organized the implementation and evaluation of the experiment and performed statistical analysis of the results. GL and JB discussed the results and prepared the manuscript. GL wrote the first draft of the manuscript. Both authors designed the concept of the research attempt and undertook identification of the fungi.The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.All claims expressed in this article are solely those of the authors and do not necessarily represent those of their affiliated organizations, or those of the publisher, the editors and the reviewers. Any product that may be evaluated in this article, or claim that may be made by its manufacturer, is not guaranteed or endorsed by the publisher.


Orange sweet potato (OSP) and red rice (RR) are rich sources of health benefit-associated substances and can be conventionally cooked or developed into food products. This research approach was to closely monitor the changes of bioactive compounds and their ability as antioxidants from the native form to the food products which are ready to be consumed. Moreover, this research explored the individual carotenoids and tocopherols of raw and cooked OSP and RR and their developed flake products, and also investigated their antioxidant activity, physicochemical properties, and sensory properties. Simultaneous identification using the liquid chromatographic method showed that OSP, RR, and their flake products have significant amounts (µg/g) of β-carotene (278.58–48.83), α-carotene (19.57–15.66), β-cryptoxanthin (4.83–2.97), α-tocopherol (57.65–18.31), and also γ-tocopherol (40.11–12.15). Different responses were observed on the bioactive compound and antioxidant activity affected by heating process. Meanwhile, OSP and RR can be combined to form promising flake products, as shown from the physicochemical analysis such as moisture (5.71–4.25%) and dietary fiber (13.86–9.47%) contents, water absorption index (1.69–1.06), fracturability (8.48–2.27), crispness (3.9–1.5), and color. Those quality parameters were affected by the proportions of OSP and RR in the flake products. Moreover, the preference scores (n = 120 panelists) for the flakes ranged from slightly liked to indifferent. It can be concluded that OSP and RR are potential sources of bioactive compounds which could act as antioxidants and could be developed into flake products that meet the dietary and sensory needs of consumers. Modern food trends and lifestyle changes have strongly influenced the dietary habits of society. The demands for ready-to-eat and simple-to-prepare foods are increasing rapidly, providing an excellent opportunity for food industries to play a significant role in supplying such food products. Flakes, one of the most popular foods made from cereals, typically oat, corn, and barley, are commonly served for breakfast with milk in Europe and the USA, and their global appeal is gaining traction. In addition, healthy eating has become a new trend in modern culture, with consumers increasingly opting for healthy food options. Secondary metabolites found in plants have been shown to decrease the risks of degenerative diseases such as coronary heart disease, diabetes, cancer, and stroke ,2,3,4. TOryza nivara L.) is a variety of rice with red pericarp caused by anthocyanins in the aleurone layer. It is a rich source of anthocyanins such as cyanidin 3-O-glucoside and peonidin 3-O-glucoside /g. In addition, methanol was used for the reagent blank.The ferric reducing antioxidant power (FRAP) was examined based on a previously published report . In brieA previous report  was follThe moisture content was measured thermogravimetrically . In brieThe water absorption index was examined according to previously published method . In briey-axis at the graph’s highest point is the maximum force value that can be held by the sample, called the value of fracturability. Crispness can be measured through changes in displacement distance during a drastic decline in the graph pattern from the highest peak to the next peak point. Meanwhile, the color profiles of flakes were measured using color reader Konica Minolta CR-10 . The results were expressed as Lightness (L*), redness (a*), yellowness (b*), ohue (oh), and Chroma (C).The fracturability and crispness of flakes were measured using TA-XT Plus Texture Analyzer  . The proThe sensory evaluation was conducted by 120 untrained panelists to determine the level of consumer preference for the flakes with various proportions of OSP and RR. The parameters tested were preferences for color, taste, crispness of flakes, and mouthfeel when served with milk. The Hedonic Scale Scoring method (preference test) with a scale ranging from 1 (strongly disliked) to 7 (strongly liked) was used for the sensory test. Samples of flakes for the color preference test were prepared in open white plastic containers. Panelists were asked first to assess aspects of flakes’ taste, color, and crispness before serving with milk. The crispness was evaluated based on the panelist’s preference for the sound of flakes during biting. For the mouthfeel test, 5 g of flakes were prepared in a small plastic container. Panelists were instructed to pour 10 mL of milk into the container and wait for 1 min. Then, they were asked to assess the mouthfeel of the flakes based on preference level by filling the questionnaire sheet provided. The data were statistically analyzed using ANOVA (α = 5%) followed by Duncan’s Multiple Range Test (DMRT) on SPSS software version 19. Spider web chart analysis using Microsoft Excel was used to determine the best proportion of OSP and RR in flakes based on the panelists’ preferences.Interestingly, the flakes with 100% RR showed a higher phenolic content than the cooked RR. Anthocyanin was only observed in RR. Furthermore, flakes containing 100% RR had a lower anthocyanin content than the conventionally cooked RR.Of the carotenoids, OSP had a higher content of β-carotene, α-carotene, β-cryptoxanthin, and lutein. β-carotene and β-cryptoxanthin were the dominant carotenoids observed in RR. The cooking process significantly decreased the content of β-carotene in OSP and RR by roughly 48% and 56%, respectively. Overall, flakes containing higher amounts of OSP showed higher carotenoid contents. The processing significantly decreased the carotenoids in the flake products when considering the raw forms and the proportions of OSP and RR, and β-carotene was the major carotenoid remaining in the flake products.Moreover, raw RR contained higher α-tocopherol than OSP in raw forms. Unlike the decreasing trend observed in other bioactive compounds due to processing, the tocopherol and α-carotene contents of both RR and OSP increased after conventional cooking. On the other hand, the two-step thermal processing decreased the tocopherol content of flakes.The antioxidant activity of raw and cooked OSP and RR and their flake products were examined using DPPH, FRAP, and Superoxide radical scavenging activity methods. The proportion of OSP and RR in the flake formulation affected the moisture content of flakes. A lower OSP proportion resulted in a lower moisture content of flakes . The dieThe water absorption index of flakes was lowest at an OSP to RR ratio of 40:60, with 0.96 ± 0.03%, and was generally higher at combination ratios of 100:0, 80:20, 0:100, and 20:80. In addition, the texture characteristic of flakes was determined by the fracturability and crispness. The highest fracturability value was found in flakes made from 100% OSP (8.48 ± 0.09). The reduction of the OSP proportion in flakes caused a decrease in fracturability until the proportion of 40:60 (2.27 ± 0.04), beyond which the fracturability of flakes increased. A similar trend was observed in the crispness value of flakes. The lowest crispness value was detected in flakes with an OSP to RR ratio of 60:40, while higher values were obtained at ratios of 100:0, 0:100, 20:80, and 80:20.Furthermore, the color of flakes was affected by the color of OSP and RR. The color profile of the flakes is shown in A preference test was conducted to determine the sensory characteristics of the flakes. The results are presented in Phenolic compounds are the most widely found bioactive compounds in plants . Some arHere, cooking led to a 49% decrease in the phenolic compounds of RR. Heating of RR generally destroys the structure of phenolic compounds by breaking the esterified and glycosylated bonds, thus decreasing the quantified content of phenolic compounds in cooked RR . Our resA similar trend was observed in the anthocyanin content of RR. The cooking process resulted in a significant decrease in the anthocyanin content due to the unstable property of anthocyanins when exposed to high temperatures . AnthocyMoreover, there is a growing research interest in the conversion of β-carotene and α-carotene absorbed in the duodenum to retinol by intestinal enzymes . The higVitamin E deficiency could lead to severe neurological problems. The main vitamin E compounds are tocopherols, with both α- and γ-tocopherol providing most vitamin E activity. Both samples had high contents of α- and γ-tocopherol. A significant increase (74%) in α-tocopherol was found in OSP after boiling. This result indicates that heat treatment could be beneficial for the bioaccessibility of tocopherol. Furthermore, heat treatment can assist in the breakdown of complex foods. Thus, tocopherol can be quickly released from its binding site. On the contrary, heat treatment was reported to reduce the tocopherol content in corn . The incThis research measured the antioxidant activity of raw and cooked OSP and RR and their flake products using DPPH, FRAP, and Superoxide radical scavenging capacity assays. The result showed that heat treatment was responsible for decreasing the antioxidant activity of OSP, RR, and the flake products. A positive correlation was observed between the reduction of bioactive compounds and antioxidant capacity. Most bioactive compounds are heat sensitive, which influences their antioxidant activity. A previous study reported that an increase in temperature accelerated the initiation of oxidation, preventing antioxidant compounds from working optimally . The bioRegarding the physicochemical and sensory properties of the flakes, it was observed that the moisture content of flake products was mainly influenced by their composition. Starch is the dominant carbohydrate found in OSP and RR, and OSP has a lower amylose content compared to RR. According to Wang et al. , the amyThe dietary fiber content of the flakes ranged between 9.47 and 13.86%, comparable to values commonly found in breakfast cereals such as corn flakes, rice, quinoa, millet, and amaranth flakes . The proWater absorption index (WAI) is a physical property associated with the ability of flakes to absorb water molecules within a particular time. Absorbed water molecules could be bound or detained in matrix pores of flakes. The water absorption index is crucial because it is associated with the quality of the flakes. Consumers can experience the crispy and crunchy sensation of the flakes after soaking in milk or water. In contrast, the higher WAI is interrelated with the unwanted soggy texture of flakes. The WAI is influenced by the porosity of the matrix on flakes, thickness, and hygroscopicity of flakes. In addition, the presence of fiber and protein could assist the flakes in absorbing water into their structure. The result shows that increasing the proportion of RR reduces the WAI due to a decrease in hygroscopicity. OSP is a rich source of sugar; thus, it has higher hygroscopicity compared to RR. In addition, the presence of RR affects the network construction of flakes by inhibiting the formation of the starch–protein structure, which could entrap gas. The compact structure created by RR starch inhibits water absorption into the matrix of the product. On the other hand, RR has higher fiber and protein contents, which help improve water absorption . MoreoveFracturability is a physical property related to deformation conditions when a specific maximum force is applied. A higher fracturability value represents the ability of food products to maintain their structure when force is applied. According to The color profile shown in The sensory analysis involved a preference test of the color, taste, crispness, and mouthfeel. Flakes containing 100% OSP had the lowest color preference score, associated with the orange appearance, and the lowest brightness score. Most panelists perceived the dark orange color as less fresh, less attractive, and less tasty. The color preference was increased with the addition of RR, which also helped improve the product lightness and redness values. The panelists were mostly in favor of flakes that appeared brighter and reddish. The higher brightness level is attributed to the white endosperm color of RR, while the redness is related to the anthocyanins in the bran of RR. The mouthfeel preference of flakes is associated with the water absorption index. The higher the ability of flakes to absorb water, the greater the plasticizing effect due to the presence of more hydrophilic components such as the phosphate monoester found in sweet potato starch . The panThis research successfully monitored the changes of the bioactive compound and antioxidant activity of OSP and RR in their native form and in the flake products. It can be observed that individual compounds acted differently to processing methods. Therefore, it can be suggested that research on the development of functional foods should address the products ready to be consumed instead of solely focusing on the raw materials due to the changes that take place during the transformation. This approach should be implemented for other potential materials rich in bioactive compounds. Moreover, further consideration of the bioaccessibility and bioavailability that are affected by digestion and absorption in the human metabolism system should also be considered .OSP and RR are rich sources of bioactive compounds, especially β-carotene, for OSP, and phenolic compounds and anthocyanins, for RR. The boiling process significantly decreased most of the bioactive compounds, except tocopherols and α-carotene. The level of bioactive compounds in the flake products was dependent on the proportion of OSP and RR. Heat treatment resulted in a decrease in antioxidant activity, even though the remaining activity was still considerably high. The mixture of OSP and RR can produce flakes with low moisture and high fiber contents. The optimum flake water absorption index, fracturability, and crispness were obtained by combining 40% OSP and 60% RR. Moreover, the ratio of OSP and RR influenced the color and sensory preferences of the panelists.


The spine has a complex motor control. Its different stabilization mechanisms through passive, active, and neurological subsystems may result in spinal stiffness. To better understand lumbar spinal motor control, this study aimed to measure the effects of increasing the axial load on spinal stiffness.A total of 19 healthy young participants  were assessed in an upright standing position. Under different axial loads, the posterior-to-anterior spinal stiffness of the thoracic and lumbar spine was measured. Loads were 0%, 10%, 45%, and 80% of the participant’s body weight.p < 0.001]. Vertebrae and loading had no interaction . Post hoc tests using Bonferroni correction revealed no changes with 10% loading (p = 1.000), and with every additional step of loading, spinal stiffness decreased: 0% or 10–45% loading (p < 0.001), 0% or 10–80% loading (p < 0.001), and 45–80% (p < 0.001).Data were normally distributed and showed excellent reliability. A repeated-measures analysis of variance with a Greenhouse–Geisser correction showed an effect of the loading condition on the mean spinal stiffness [F  = 3.456, We conclude that a load of ≥ 45% of the participant’s body weight can lead to changes in the spinal motor control. An axial load of 10% showed no significant changes. Rehabilitation should include high-axial-load exercise if needed in everyday living. A well-working spinal motor control system is needed to protect the human spine from injury and to prevent low back pain  induced by parabolic flights . The remaining lumbar and thoracic spinous processes were located by counting from L5 and marked with ink.Posterior-to-anterior lumbar and thoracic spinal stiffness was assessed in one session. Before data collection, the procedure was explained to the participant, and one familiarization test measurement was performed. Thereafter, the first two measurements were performed with no axial load in a normal upright standing position. Then, two measurements with 10%, 45%, and 80% of their body weight as an additional load were conducted, resulting in eight measurements. The 10% and 80% loading were chosen based on the literature  impulse  with spinal stiffness as a dependent variable and different loads as a within-participant factor was used. Vertebral levels (T3–L5) were used as a continuous covariate. Post hoc testing using Bonferroni correction was used. Data were collected and stored using REDCap . For statistical analysis, SPSS 25  was used.A total of 19 participants were recruited . No participant had to be excluded, and no participant felt pain during or after any of the measurements. Table p < 0.021]. No significant interaction was observed between the vertebral level and loading . Post hoc tests using Bonferroni correction revealed that with 10% additional axial load, stiffness remained unchanged (p = 1.000). With every additional step of loading, spinal stiffness significantly decreased: 0%/10–45% loading (p's < 0.001), 0%/10–80% loading (p's < 0.001), and 45–80% (p < 0.001). All mean and standard deviation stiffness values can be found in Table The Shapiro–Wilk test indicated a normal data distribution in all loading conditions (p's = 0.130 (no loading)/0.616 (10% load)/0.676 (45% load)/0.819 (80% load)). A repeated-measures ANOVA with a Greenhouse–Geisser correction showed a significant effect of loading condition on mean spinal stiffness [F 2.6, 744) = 3.456, .6, 744 =This study showed decreased spinal stiffness when the additional axial load was equal to or greater than 45% of the participants’ body weight. Conversely, no change was observed with an additional load of 10% of the body weight.Decreased lumbar spinal stiffness with higher axial loads might be the result of the changes in the lumbar motor control strategy (Swanenburg et al. In contrast to the results for additional axial loads of ≥ 45% of the participants’ body weight, no changes in stiffness were observed for the 10% additional load in this study. A study on participants carrying a backpack weighing between 15 and 30% of their body weight showed only a minimal increase in abdominal forces (Goh et al. Spinal stiffness in in vivo evaluations should be noted to include measurements of all subsystems, and the measured value represents the net effect of all combined subsystems. As this makes in vivo measurements of spinal stiffness ecologically relevant, no information with respect to individual subsystems is obtained. Thus, the stiffness of the passive subsystem also possibly increased in this study, as shown in the in vitro study (Edwards et al. The results of this study of a possible change of spinal motor control might be particularly interesting from a clinical point of view. Nonfunctioning motor control of the spine can affect the alignment of the lumbar spine segments, resulting in considerable strain on the lumbar spine (van Dieen et al. Participants’ arms were hanging along the torso when measuring spinal stiffness with no additional load. When the additional load was fixed, the hands were placed at the weight bar, which was laid over the shoulder. Lifting the arms leads to an increased shoulder muscle activity, which, in turn, results in increased spinal stiffness (Escamilla et al. This study found that a load of ≥ 45% of the participant’s body weight can lead to spinal motor control changes, whereas an axial load of 10% showed no significant changes. Rehabilitation should include high-axial-load exercise if needed in everyday living.


Zirconia repair could be a feasible alternative option to total replacement in fractured zirconia-based restorations. Maximising the bond strength by enriching zirconia with fluorapatite glass-ceramics (FGC) powder has been addressed and compared to other surface treatments. Besides resin composite, other repair materials have been proposed and compared. Zirconia blocks received different surface treatments . B—sandblasting with FGC powder (FGC), C—fluorapatite glass-ceramic coat+ neodymium-doped yttrium aluminum garnet laser irradiation (FGC + Nd: YAG), and D—no surface treatment). The surface roughness, topography, and crystallinity were investigated by a profilometer, scanning electron microscopy (SEM), and X-ray diffraction (XRD) analyses, respectively. For each surface treatment, three repair materials  were bonded to zirconia with 10, Methacryloyloxydecyl dihydrogen phosphate (MDP)–Monobond Plus/ Multilink Automix. Bonded specimens were thermocycled for 10,000 cycles and tested for shear bond strength (SBS) at a speed of 1 mm/min, followed by the analysis of the mode of failure. FGC + Nd: YAG laser group reported the highest surface roughness and monoclinic content compared to CoJet, FGC, and control groups. The highest mean SBS was found in FGC-blasted zirconia, followed by FGC + Nd: YAG laser and CoJet treated groups. However, the lowest SBS was found in control groups regardless of the repair material. Sandblasting zirconia with FGC powder increased SBS of resin to zirconia with lower monoclinic phase transformation compared to FGC + Nd: YAG or CoJet groups. Zirconiorations . Zirconiorations ,5. Unfororations . Heintzeorations . The comorations .Repairing fractured ZBR would be an attractive option for a cost-effective and time-saving approach instead of total replacement ,9,10. ThEstablishing a durable bond between repair material and zirconia is questionable. In glass-ceramics, hydrofluoric acid etching (HF 9%), followed by a silane application, has been the routine mechanical and chemical treatments to modify the surface topography and enhance the bond strength of glass-ceramics to resin composites, respectively. HF attacks the glassy matrix of glass-ceramics and creates micromechanical locks for resin bonding . The absFluorapatite glass-ceramics (FGC) has been recently used as a veneering material to zirconia core. It showed to be compatible with zirconia with reported higher shear bond strength than veneering feldspathic glass-ceramics . IPS e.mFollowing sandblasting, priming zirconia surface with phosphate monomer 10- methacryloyloxydecyl dihydrogenphosphate (10-MDP) has been considered the next key step for a durable repair of ZBR. 10-MDP is a phosphate monomer with bifunctional molecules that chemically bond to zirconia and resin composite ,20.Dental lasers, such as neodymium-doped yttrium aluminium garnet (Nd: YAG), have been widely applied in dentistry for different dental procedures; treatment of hypersensitivity, cavity preparations, and office bleaching, to name a few . Nd: YAGIn the current study, zirconia has been coated with FGC powder followed by Nd: YAG laser irradiation (FGC + Nd: YAG) as an attempt to increase the surface content of zirconia with glass-ceramics. FGC + Nd: YAG is a modified approach to silica-lasing, in which a lab-prepared FGC powder, instead of a slurry of feldspathic porcelain, was used followed by Nd: YAG laser irradiation at a power of 4 W. It is believed that laser power will melt down the FGC particles down to the zirconia surface. However, this hypothetical interaction has never yet been tested and verified.Therefore, the current study investigated the effect of sandblasting with FGC powders or tribochemical silica-coated alumina and FGC + Nd: YAG approaches on shear bond strength (SBS) of different repair materials  to zirconia. The null hypotheses tested were (i) different surface treatments would not affect SBS of different repair materials to zirconia and (ii) different repair materials would not significantly change the SBS to zirconia.A total of 20 partially sintered IPS e.max ZirCAD MO  zirconia blocks (15 mm × 19 mm × 55 mm) were cut into 120 zirconia blocks of 15 mm × 19 mm × 6 mm using a precision diamond saw IsoMet 1000 , as illustrated in A mortar and pestle were used for crushing down the fluorapatite glass-ceramic ingots  into smaller frits with an average size <5 mm. Each 1 g of the crushed frits was further pulverised using a mixer mill  at parameters of 20 Hz for 1 min. The particle size of the obtained powders was measured using a laser diffraction particle size analysis .Zirconia blocks were randomly assigned to four groups of 30, one of which worked as a control group.Group A (CoJet): The surface of zirconia specimens were airborne-particle abraded using an intraoral microblasting unit  with 30 μm silica-coated alumina particles  at 3 bar pressure for 15 s at 10 mm distance ;Group B (FGC): Zirconia blocks were sandblasted using the ground FGC (IPS e.max ZirPress) powder (53 µm) using sandblasting unit  for 15 s under a pressure of 3 bar at a distance of 10 mm;Group C (FGC+ Nd: YAG): Zirconia surfaces were covered by a custom-made brass metal with central perforation exposing a circular area of zirconia with a diameter of 5 mm. FGC powders were mixed with distilled water and brushed over the exposed zirconia surface using a paintbrush. They were left to dry before Nd: YAG laser irradiation  was applied perpendicular to zirconia at 1mm away, as illustrated in Group D (Control): As polished.One specimen from each group was used for surface topography investigation. Specimens were platinum coated and viewed using a scanning electron microscope  with an accelerating voltage of 10 kV and a working distance of 8.5–9 mm. Secondary electron images were taken at a magnification of 2000×, followed by energy dispersive spectroscopy (EDS) for elemental analysis. A total of 40 zirconia specimens (N = 10) were used for surface roughness evaluation by a contact stylus profilometer . Stylus probe with a radius tip of 2 µm and contact force of 0.7 mN travelled a length of 4 mm in the centre of the treated zirconia at speed of 0.5 mm/s, and a cut-off value of 0.08 mm. Five readings, in parallel lines, were measured per specimen. The following roughness parameters were calculated: (i) the arithmetic average of surface profile (Ra), (ii) the maximum average of the highest peak and lowest valleys (Rz), (iii) an average of maximum peaks (Rp), and (iv) the average of deepest valleys (Rv).α X-ray tube head (λ = 1.5416 Å) operated at 40 kv and 30 mA with scanning speed of 12°/min, step size of 0.02° and 1 s/step. XRD peaks were collected at a 2-theta range between 5° to 80°. Phase identification of tetragonal and monoclinic zirconia was conducted using the Shimadzu Xlab software program  and compared with the International Centre for Diffraction Data (ICDD) XRD database. The amount and volume fraction of the monoclinic zirconia phase were calculated according to Garvie and Nicholson equation [XM is the monoclinic peak intensity ratio in sandblasted zirconia; VM is the volumetric fraction of monoclinic phase in sandblasted zirconia. The zirconia phase transformation from tetragonal to monoclinic, as for the blasted and control groups, was investigated using an XRD diffractometer  with Cu Kequation  modifiedequation .(1)XM =TM 13  were obtained using a custom-made brass mould with inner dimensions of 5 mm diameter and 3 mm in thickness. Feldspathic powder and modelling liquid were mixed using a plastic spatula until the mix was homogenous with a dough-like consistency. The mould was then loaded by the mix and excess liquid was removed by absorbent tissue. A key was then used to dislodge the specimens from the mould. All the specimens were then sintered in a porcelain oven  following the manufacturer’s instructions, as illustrated in A total of 40 cylinders (5 mm diameter and 3 mm thickness) of feldspathic porcelain VITAVMFeldspathic porcelain undergoes ≈20% volumetric sintering shrinkage. For this reason, specimens were returned to the mould and a mixture of porcelain powder and the liquid was added again and then another firing cycle was carried out. Sharp edges were removed using a diamond disc mounted on a low-speed handpiece. Specimens were then finished and polished with P1000 and P1200 silicon carbide papers using grinding machine Metaserv 250 .Lithium disilicate porcelain  is presented in form of rectangular blocks to be milled by a CAD/CAM machine. The rectangular blocks were trimmed into a cylindrical shape with a diameter of 3 mm using a milling machine. A total of 40 cylinders (5 mm in diameter and 3 mm in thickness) of lithium disilicate porcelain were then obtained by sectioning the milled IPS e.max CAD cylinders using Isomet 4000  at speed of 300 rpm, as illustrated in The surface area of bonding for each zirconia specimen was defined using a pre-perforated adhesive tape covering the zirconia surface exposing only a well-circumscribed round area of 5 mm in diameter. For each surface treatment, repair materials were assigned into three subgroups (n = 40/subgroup) as follows:Tetric: Adhese Universal + Monobond Plus + Tetric EvoCeram Bulk Fill;TM 13;VM 13: Monobond Plus + Multilink Automix + VITAVM IPS e.max CAD: Monobond Plus + Multilink Automix + IPS e.max CAD.a-2. Custom-made silicone mould with a 5 mm diameter and 3 mm thickness was then placed over the bonding area. The mould was then bulk-filled by Tetric EvoCeram Bulk Fill using a plastic filling instrument before it was light-cured for 20 s.For the Tetric group, zirconia surfaces were rubbed with 10-MDP Monobond Plus for 1 min and air-dried for 5 s before coated with Adhese Universal using microbrush and light-cured for 10 s using a LED curing light  with an output of irradiance of 1200 mW/cmb-For VM 13 and e.max CAD groups, exposed zirconia was treated with 10-MDP Monobond Plus and left for 60 s and then air-dried for 5 s. VM13 and IPS e.max CAD specimens were etched with  for 1 min, water-rinsed, and air-dried before they were treated with Monobond Plus primer for 1 min. Multilink Automix resin cement was extruded over the bonding area using a double syringe through an auto-mixing tip.For all groups, a mass of 2.25 kg was applied on the top of each resin composite specimen for 5 min to allow the flow of excess resin . Excess 2). The bonded resin composite cylinders to zirconia blocks for all groups were mounted into a jig and the shear bond strength was measured using a Universal Testing Machine  with a knife-edge shearing rod in a load cell capacity of 5000 N at a crosshead speed of 0.5 mm/min b. The ma(A)adhesive failure: Failure between the resin composite and zirconia surface;(B)mixed failure: Combined adhesive and cohesive failure in resin composite specimen.The mode of failure of debonded specimens was evaluated under SEM . Failure modes were assigned to be  as folloSurface roughness and SBS values were analysed using SPSS for Windows version 22.0 . The normal distribution of data was explored using Kolmogorov-Smirnov’s test. Data on surface roughness analysis and SBS were found to be normally distributed. Thus, one-way ANOVA was conducted to compare mean values of surface roughness parameters of studied zirconia groups, while two-way ANOVA was used to test SBS, as a dependent variable, on the interaction effect of both surface treatment and repair materials as independent variables. Tukey post hoc test for multiple comparisons was subsequently used to compare the mean SBS between studied groups to detect the statistical difference at a level of significance α = 0.05.This section may be divided by subheadings. It should provide a concise and precise description of the experimental results, their interpretation, and the experimental conclusions that can be drawn.Images of the scanning electron microscope (2000×) for the tested zirconia surface are presented in EDS analysis of the percentage mass of silica for differently treated zirconia groups is presented in p > 0.05). No significant difference was detected in the Rp value between the control and CoJet groups, while the Rp of the FGC group was statistically higher than the control and CoJet groups. The mean Rv value of FGC was higher than the control group with no significant difference compared to that of CoJet that was significantly higher (p < 0.05). Mean Rz values were the lowest in the control group followed by CoJet and FGC groups with a statistical significance found (p < 0.05). However, no significant difference was found in Rz between CoJet and FGC. Generally, the FGC + Nd: YAG group recorded the highest statistically significant values of mean Ra, Rp, Rv, and Rz compared to the rest of the groups (p < 0.05).Descriptive statistics of surface roughness parameters and one-way ANOVA results are summarised in T -101) was the most accentuated in Group D and most reduced in Group A. Broadening of the tetragonal peak was noticed in treated zirconia surfaces indicating the presence of rhombohedral phase or distorted tetragonal phase.Diffraction peaks are presented in Mean SBS values of studied groups and two-way ANOVA statistical comparison were shown in p = 0.00) compared to the previous two surface treatments except for zirconia samples repaired with Tetric EvoCeram Bulk Fill. Control groups showed the lowest values for different repair materials, except for IPS e.max CAD- repaired zirconia.Generally, sandblasting zirconia with FGC powders showed the highest mean SBS, followed by FGC + Nd: YAG approach for different repair materials. CoJet sandblasting reported significantly lower mean SBS (TM 13 and Tetric EvoCeram Bulk Fill) regardless of the surface treatments applied.IPS e.max CAD showed the highest mean SBS compared to the other two repair materials (VITAVM p > 0.05), while CoJet sandblasting and no surface treatment significantly lowered the SBS for the same repair material .The highest mean SBS was found in zirconia specimens treated with FGC sandblasting and repaired with IPS e.max CAD (36.4 ± 2.3 MPa), followed by FGC + Nd: YAG treated group (35 ± 2.2 MPa) with no statistical difference  compared to VITAVMTM 13 (14.2 ± 2.1 MPa).For the same surface treatment, there was no statistically significant difference between Tetric EvoCeram Bulk Fill and VITAVMp < 0.05) on the shear bond strength values obtained. Repair materials used had a more impact on SBS values than the surface treatment employed.Two-way ANOVA showed that each of the independent variables  or both together had a statistically significant effect (TM 13). However, combined failure in all specimens was found in the FGC group repaired with either of Tetric EvoCeram Bulk Fill or IPS e.max CAD. The same mode of failure was also found in CoJet-sandblasted zirconia repaired with VITAVMTM 13.Modes of failure are represented in TM 13 to 40% in zirconia repaired with IPS e.max CAD.In group C, adhesive failure ranged from 20% in the zirconia group repaired with VITAVMSEM images  showed aChipping and delamination of the veneering porcelain are the most common mechanical failures of ZBR . After fSEM images showed the impact of surface treatments on changing the surface topography of zirconia. The hypothesised interaction between FGC particles and zirconia upon blasting or laser fusion has been confirmed in the current study through the EDS analysis. Progressive increase of silica content from CoJet group (1.25 ± 0.13%), followed by FGC and FGC + Nd: YAG groups  was found. These results are consistent with the findings of a previous study [Surface roughness parameters showed the significant impact of FGC + Nd: YAG on zirconia surface compared to other groups. This finding is consistent with previous studies ,32,33. HXRD pattern showed the presence of monoclinic phase in all zirconia specimens, including the control group, and broadened tetragonal peaks for the other groups. The monoclinic phase was found in the as-sintered zirconia (control) in previous studies ,36,37. SShear bond strength (SBS) is a simple and reliable testing method to investigate bond strength between dissimilar materials, especially when the bonding surface area has an average diameter of 5 mm . It was Sandblasting zirconia with silica-coated alumina particles creates surface microretentive areas and enriches zirconia surface with silica in a process called silicatisation . SilicatAlumina-free glass-ceramics have been compared to the conventional silica-coated alumina to blast zirconia in a previous study . AuthorsFGC + Nd: YAG is an alternative approach that hypothesised an effective mechanical roughening to zirconia with the potential fusion of FGC powder into the surface. The effect of this approach has been investigated and compared to other surface treatments for the first time in the current study. FGC + Nd: YAG approach reported non statistically significant lower SBS compared to FGC sandblasting regardless of the repair material . Nd: YAGCoJet sand has been a successful sandblasting approach that reported mean SBS of resin composite to zirconia ranging from 17.16 ± 1.19 MPa  to 22.9 p < 0.05) in all surface treatments. This finding is consistent with Yilmaz et al. [1/ [Lithium disilicate (IPS e.max CAD) has been used as a potential repair material for zirconia in the current study. The results showed that IPS e.max CAD has reported the highest mean SBS (36.43 ± 2.3 MPa) compared to the other repair materials with statistical significance  compared to Tetric EvoCeram Bulk Fill resin composite (21.48 ± 2.06 MPa), which is in agreement with [Feldspathic porcelain (VITA VM13) has been used in the current study as a repair material, in addition to resin composite, for fractured ZBR. The results of our study showed a maximum SBS of 20.30 ± 2.22 MPa in the FGC group with no statistically significant difference (ent with . The selent with ,76. It hent with . Furtherent with . HoweverHowever, this in-vitro study investigated one type of zirconia substrate with the application of one primer/adhesive and employed single parameters of one laser device. Different laser devices and parameters, other types of zirconia substrates, and primers/adhesives should also be tested to provide a more concise prediction of how laser power can be an effective alternative approach in zirconia repair protocols.It is concluded that t-m phase transformation depends on the surface treatment employed, where blasted zirconia with CoJet sand or Nd: YAG laser treatment to FGC-coated zirconia revealed the highest number of monoclinic crystals compared to FGC-blasted zirconia. Laser-fused FGC showed the highest surface roughness to zirconia compared to FGC or CoJet. FGC-blasted zirconia reported a higher amount of silica compared to CoJet sand and contributed to a significant increase in the shear bond strength of either feldspathic porcelain or lithium disilicate to zirconia. Sandblasting zirconia with FGC powders and FGC + Nd: YAG could be effective alternative approaches for zirconia repair. While direct resin composite and feldspathic porcelain could work as repair materials for fractured ZBR, lithium disilicate might be a better choice especially when high mechanical properties are a prerequisite.


When starch was phosphorylated with Na2HPO4, HVED was more efficient in catalyzing reaction , whereas with Na5P3O10 similar P content was achieved as with thermal treatment (0.76 P/kg for 30 min HVED in relation to 0.86 mg P/kg). The order of HVED and chemical reactions did not have a marked effect on phosphorous content. In combination with Na2HPO4, HVED pre-treatment had a more pronounced effect on the solubility and water absorption, whereas post-treatment was favoured with Na5P3O10. Mean diameter was increased by all treatments, where HVED had a marked effect. Enthalpy of gelatinization ranged from 11.76 J/g for starch treated with Na5P3O10 and 10 min-HVED to 13.58 J/g for Na5P3O10 treated sample. G′ and G″ increased after both thermally and HVED enhanced phosphorylations, with a slightly more pronounced effect of the HVED.The aim of this research was to explore the use of a high-voltage electrical treatment (HVED) as a substitute for heating during the phosphorylation of maize starch. Starch was treated with HVED, phosphorylated with Na Starch is found in numerous food products, from bread to yoghurt, where it has thickening, gelling or texture improving functions. Gelatinisation, rheological properties, water absorption and solubility of starches are important parameters for the evaluation of the effect of starch on food properties. Native starches often do not fulfil all the requirements for specific use in foods. Most often, they are not stable enough at high temperatures, in acidic conditions, during storage, or do not gelatinise at required temperatures and do not have desired rheological properties. In order to obtain the optimal effect and optimal aforementioned properties, starch has to be modified, which is most often done by chemical reactions .Phosphorylation is a commonly applied modification procedure that requires a thermal treatment at high temperatures (130 °C up to 160 °C) in order to maximize the reaction efficiency. Generally, starch phosphates are prepared using sodium dihydrogenphosphate, disodium hydrogenphosphate , sodium Since the process commonly requires high energy consumption and may result in undesired changes, such as colour degradation, deterioration of structure and formation of free radicals , a high-To this day, HVED has been applied as an extraction technique , decontaThe aim of this research is to examine if HVED may be used as an aid in phosphorylation of starch, instead of the thermal treatment, with phosphorus content and properties similar to the starch modified in classical manner. 2 9.9; protein 0.5 g/100 g; fat 1 g/100 g; ash 0.1 g/100 g) was supplied by Cargill, Minneapolis, MN, USA. Na2HPO4 (p.a.) (CAS: 144-55-8) was supplied by T.T.T. d.o.o. Sveta Nedjelja, Croatia and Na5P3O10 (p.a.) (CAS: 7758-29-4) was from Acros Organics, Geel, Belgium.Native maize starch  were suspended in 200 mL of demineralised water with stirring at a magnetic stirrer for 30 min. The suspension was then centrifuged at 3000 rpm for 5 min , water was discarded, starch was washed three times with water (with centrifuging), and air-dried. Modification with NaRama Rao  with sliFor thermally treated phosphorylated starch, after the first centrifuging starch was air-dried overnight and thermally treated at 130 °C/2 h. Starch was then suspended in 250 mL of water, centrifuged, and washed three times with water. The obtained starch was dried at ambient temperature. 5P3O10 was done according to Lim and Seib [5P3O10 and 2.5 g of Na2SO4 was dissolved in 200 mL demineralized water. An amount of 100 g of starch was suspended in the solution by stirring at a magnetic stirrer for 20 min. pH of the suspension was set to 10.0 by drop-wise adding of NaOH (0.45 M) and the suspension was stirred for another hour. The suspension was centrifuged at 3000 rpm for 5 min , water was discarded and starch was washed three times with water, and air-dried.Phosphorylation with Naand Seib  with andFor thermally treated phosphorylated starch, after centrifuging, starch was roasted in the oven at 130 °C/2 h, washed three times with water, and air-dried.HVED device used in this research was custom-made by Ingeniare CPTS1, Osijek, Croatia and is described in more detail in Barišić et al. . An amouCombined treatments were conducted by the HVED treatment for 10 or 30 min prior to the phosphorylation and vice-versa. For combined treatment, drying at 130 °C was omitted in order to explore if HVED may be used as a substituent for thermal reaction.The sample was prepared as described in PN-EN ISO 3946: 2000 and phosphorus was determined by ICP-OES.3 of concentrated nitric acid (V) p.a. and 1 cm3 of concentrated hydrogen peroxide p.a., then the samples were mineralized in the microwave MARS 5  sample preparation system. The minerals were quantitatively transferred to 10 cm3 measuring vessels with redistilled water. An appropriate amount was taken for the determination of phosphorus. In brief, the samples were digested "wet" in a closed microwave system with 5 cmPhosphorus was determined by induced plasma atomic emission spectrometry—ICP-OES using the ICP-AES iCAP 7400 atomic emission spectrometer . The results were confirmed using the certified reference material NCS ZC 73012 - Cabbage, and the measurement uncertainty was estimated at 5%.g. The separated supernatant was used to determine dry matter content by the gravimetric method, and the precipitate left in centrifuge tubes was weighed.Swelling power and solubility in water were determined at 80 °C, according to the method of Kapelko-Żeberska et al. . A waterMean volumetric diameter was determined as described by Gryszkin et al. , after u−1. Thermal properties were determined using the differential scanning calorimeter DSC 822E , following methodology provided by Zieba, Szumny and Kapelko , with mo−1, were determined according to Zieba, Juszczak and Gryszkin [The flow curves at 50 °C, with a shear rate range of 1–300 sGryszkin . The 5% −1), τ—shear stress (Pa), K—consistency coefficient (Pa∙s), KHB—consistency coefficient by Bulkley’s (Pa∙s), τ0—yield stress by Bulkley’s (Pa), τ0C—yield stress by Casson’s (Pa), ηC—Casson’s plastic viscosity (Pa∙s).The mechanical spectra of gels were obtained at 25 °C. The paste was obtained as described in the designation of the flow curves. The hot paste was placed in a measuring system (Z38AL type) of the RS6000 rheometer, then cooled and allowed to rest at 25 °C for 15 min. Measurements were taken in the linear viscoelastic range at a constant strain of 0.03 and a frequency from 0.1 to 10 Hz . Then, tp < 0.05 using Statistica® 13 and Microsoft Excell 2016.All measurements were done in triplicates. Statistical analysis of results was performed by analysis of variance and Fischer’s LSD test at It is well established that corn starch naturally contains small amounts of phosphorus, primarily linked to C-6 in amylopectin, with a smaller number that may be linked to C-2 and C-3  and in t2 formed by HVED reacted with an aromatic ring, resulting in ring-cleavage products, and Grinevich et al. [After the HVED treatment, the amount of phosphorus declined. This may be caused by the extraction in the water or the formation of complexes in which phosphorus would be “masked” during determination. Namely, Du et al.  reportedh et al.  reported2HPO4 increased the amount of P, showing that the reaction occurred, it was not significantly efficient unless thermal treatment or HVED was applied, with the major advantage of HVED treatment over the thermal treatment (2.781–3.892 g P/kg compared to 0.434 g/kg). Interestingly, if HVED treatment lasted 10 min, the efficiency of the reaction was lower when HVED was applied after phosphorylation with Na2HPO4 (3.411 g/kg in relation to 3.831 g/kg when HVED was applied prior to phosphorylation). The opposite was observed for the 30 min-treatment, where higher content of P was determined when HVED was applied after the phosphorylation (3.892 g/kg in relation to 2.781 g/kg).Although phosphorylation with Na5P3O10, the reaction was not efficient at all unless thermal treatment or HVED were applied  and the solubility (SOL), confirming that the chemical reaction did not occur or was too moderate to result in the change of these properties. When the starch was heated after the reaction, the water absorption increased several times, and the swelling power increased, although not so markedly. Ascheri, Pereira and Bastos [The same was observed by Andrade et al.  for stard Bastos  also rep2HPO4, although the increase in WA and SOL may be observed. Although the increase in swelling power and solubility of starch is primarily linked to the substitution of starch, Wongsagonsup et al. [Again, the HVED treatment was not as effective as with Nap et al.  claim thNamely, after all modifications, the average particle size increased due to the introduction of water molecules and phosphorylation.Gelatinization parameters determined by DSC are shown in The HVED treatment combined with phosphorylation generally decreased the gelatinisation enthalpy, hence, the gelatinisation was easier than for phosphorylated starches. This is also consistent with the increased WA and SOL of dual-modified starches compared to phosphorylated ones. Ascheri, Pereira and Bastos  reportedRheological models are given in 2 values, all three models fit well, although the Ostwald de Waele has an R2 value as low as 0.96 for some samples.Three models were applied to describe rheological properties: Ostwald de Waele, Herschel Bulkly and Casson. As can be seen from the Rn value determined by the Ostwald de Waele model is between 0.359 and 0.483, showing pronounced non-Newtonian characteristics of all analysed starches. While the combination of HVED with Na2HPO4 resulted in lower values of n compared to the combination of phosphorylation with thermal treatment, when the phosphorylation was done with Na5P3O10, the shear-thinning effect was more pronounced when the thermal treatment was applied compared to combination with HVED. Both K and n values are close to the ones reported by Hornung et al. [0 and KHB in the present research are significantly larger than the ones reported by Hornung et al. [2HPO4 modification resulted in larger values of τ0 compared to the thermally treated counterpart (except the sample that was modified with Na2HPO4 with subsequent 10 min HVED treatment), i.e., higher stress must be applied to the HVED treated monophosphorylated starch in order to start it to flow. The opposite was observed for the Na5P3O10 modification: higher τ0 were observed in combination with the thermal treatment.The g et al.  for whitg et al. . This in0C value of 10min-HVED treated Na2HPO4 modified starch lower than the thermally treated counterpart.Casson model does not fully confirm the yield stress determined by the Herschel–Bulkley model, with τC 0.044–0.047 Pas) < starches phosphorylated with Na2HPO4 (0.046–0.059 Pas) < starches phosphorylated with Na5P3O10 (0.056–0.086 Pas). Park, Chung and Yoo [However, in both models, the difference between the values was not statistically significant so this discrepancy is not relevant. Casson’s plastic viscosity is the measure of the final viscosity of pastes (at the end of shearing). From the values in the  and Yoo  ascribedStorage modulus (G′), loss modulus (G″) and loss tangent (counted by frequency 1Hz) (G″/G′) are shown in 2HPO4 and 0.26 for Na5P3O10). The values G″/G′ are close to 0.1 showing a formation of a gel network and the elastic nature of formed gels [G′ and G″ increased after both thermally induced and HVED enhanced phosphorylations, with a slightly more pronounced effect of the HVED compared to the thermal treatment. This is due to the formation of a strong gel network, according to Heo, Lee and Chang  and may med gels . Althougmed gels , and Heomed gels  reported5P3O10 modification, and even better results were achieved in Na2HPO4 modification. Accordingly, the investigated properties  were either similar to the thermally treated phosphorylated starches or improved in relation to them. Although additional research is needed to confirm the phenomena behind the HVED efficiency, it is presumably due to the activation of starch molecules both by energy increase and by polarization of active sites.The results obtained in the present research show that an HVED might be used as a substitute for the thermal treatment in a phosphorylation reaction, with a similar or even better effect on the reaction efficiency, visible from both the P content and the investigated properties of starches. Starches with a similar P content were obtained when the HVED was applied instead of the thermal treatment in Na


This paper attempts to pinpoint what French Red-Cross women were doing in the international exhibitions from 1867 to 1937. They engaged their energies into organizing meetings, exhibitions, and into healing, receiving awards for their work. In spite of their dual activity of exhibitors and healthcarers, they had no specific pavilion at the world fairs. They hovered between the worlds of politics and medicine as distinguished guests but without their own space. Although at the turn of the twentieth century, it was probably not surprising to notice the presence of women within the Red Cross Societies and in International Exhibitions, belonging to both institutions had not yet been considered. At first sight, they seemed both to be and not to be settled in a global environment. No iconographies represent Red Cross ladies at work in International Exhibitions. Yet, they were on Parisian sites starting from the early phase of the 1867 Universal Exhibition up until the 1937 International World Fair, the last paradigm of its kind. An intuitive thought places women from Red Cross Societies on the rescuing side in the public spaces of exhibitions all the way through this period.The issue here, other than knowing who they were, is to identify what, in the eyes of the world, they did: were they just ordinary members of nationwide societies, professional health staff who ensured the protection of visitors in international exhibitions? Or, did they carry out, in a national agenda, an International philanthropic activity, showing generosity, kindness, benevolence, help, assistance and “love of mankind” Littré, ? In otheThe involvement of French Red Cross women in International Exhibitions is an aftermath of Solférino. It brings us back to the emotion Henry Dunant (1828–1910) a philanthropist Jaeger, 1 from Ge“In the church the women of Lombardy go from one to the other with jars and pitchers full of water, which serve to appease the thirst and to bathe the wounded. Some of these improvised nurses are good-hearted old women, other are charming young girls. Their gentleness, goodness, compassion and their attentive care restored a little courage to the wounded”  took the lead of the Italian Ladies Relief Committee  started with this motto “Inter Arma Caritas” . Its main objective was to assist civilians and military who were wounded. Its members, having Catholic and Royalist backgrounds,Both doctors and women felt for their fellowmen and put a lot of effort into curing and caring. In France, the “…were to help not only their own country's sick or wounded, but also ‘all the unfortunate who fall into their hands, irrespective of nationality.’ This mutuality would ensure proper treatment for any wounded man which ever society had him in its care”  was to be remembered for praising the Marquis de Vogüé, President of the French Red Cross Central Committee, and Gustave Moynier, President of the International Red-Cross Committee, who wanted to extend “charitable activities all over the world” , Le Play's invitation was primarily the opportunity to promote their first International ConferenceIn willing to distribute awards, the I.C.R.C. was acting like the organizers of the 1867 Exhibition. It was also under pressure to take part in the world fair and displayed among 600 objects, some publications  that was solely managed by women , founded in 1881 by Mme. Koechelin-Schwartz (1838–1911), was contentedInternational Bulletin of Red Cross Societies, the need to gather together all men of humanity and charity during the world expositionAs for the other relief society the S.S.B.M, it was satisfied with the space that was allotted to it in the pavilion for hygiene and sanitary equipment  who openly stated “the higher races had duties over the lower races” Ferry, . ColoniaYet, the I.C.R.C. wished that, among the competing French relief societies, only one would correspond with the well-known General Commissioner, the Maréchal Lyautey. Thus the I.C.R.C. set an inter-society commission to make a decision and called upon their “spirit of fraternity”Therefore, in 1931, some sort of common strategy, showing a “spirit of solidarity”Femmes de France honored themselves with “privileged entries” issued by the Exhibition's commissioner. But, the inauguration day was postponed and a large number of U.F.F. members found themselves in front of closed doors of the designated pavilions.The 1931 International Colonial Exhibition not only more or less enabled the S.S.B.M., the A.D.F. and the U.F.F. to speak with different voices, but also to shed light on the U.F.F. fiftieth anniversary“[They] were only able to do a complete tour outside the building, under lashing rain; but, although they had been hardened during the war, they were nevertheless greatly interested in the show and also in explanations kindly supplied by Mr. the administrator of the colonies who showed himself willing to monitor them”The dynamism of the U.F.F. was so blatant that “they had no need  to keep in touch with their sister societies”  divided between first class nurses for curing and second class nurses for caring  that did:When visitors arrived at the Palais de Chaillot in May 1937, Spain was in the middle of civil war (see also Vilar, “… not confer the right to cure, [but] knowing effective gesturing in the case of an accident…[It was] mainly intended for all women who could not devote the proper time for studying nursing and yet who wanted to be helpful and acquired elementary knowledge in hygiene” Pineau, , p. 49.Although it was quite difficult to state precisely the content of Mme. Jobert-Dalligny's training at the U.F.F., she was definitively an experienced nurse, having spent some time in the Rabat Health Center (Chavenon, With such responsibilities, Mme. Jobert-Dalligny became the natural U.F.F. spokesperson at the 1937 International Exhibition and filled the “space for women.” She stood at a time when women's suffrage was consistently rejected and when there was an “ambiguous reflections of the question of women's rights in France Reynold, . AccordiThis 1937 experience at the World Fair stood against the already existing collaboration among International Red Cross Societies where professionalism was important. The Anglo-French-American Hospital, in Neuilly-sur-Seine, for example, was run by a Red Cross “… lady versed not only in nursing but in the practical details of organization…”But, in an International Exhibition context, the U.F.F. tended to isolate itself and opposed the worlds of medicine and politics. Women in this French Red Cross society positioned themselves primarily as distinguished guests. They were there more for the show than as a reference.Universal or International Exhibitions that took place in Paris had definitively a different impact on Women in French Red Cross Societies. If it was too early for Red Cross Ladies to invest in the first Universal Exhibition, the 1867 World Fair, held in Paris, was an opportunity to organize and structure the newly born International Relief Movement. But, the 1900 Universal Exhibition was an obstacle and a competitive place where French Red Cross Societies argued about the space they were allotted. The 1931 Colonial Exhibition worsened the relationship among French relief societies to the extent that only U.F.F. women were heard by the I.C.R.C. and held the front stage. In the history of the Red Cross Societies, the French case was peculiar in a sense that there were competing objectives. These were forecasting to a certain extent the 1940 legislation signed by the Maréchal Pétain enforcing a single French Red Cross society (Rouge, The author confirms being the sole contributor of this work and has approved it for publication.The author declares that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.


Relevant research has investigated the application of discarded oyster shell powder (OSP) replacing cement mortar and has reported certain improvements to its performance. Consequently, focusing on discovering more effects of OSP on MPC performance, this study, by using a typical three-point bending test, used 45 cuboid specimens to investigate the influences of OSP mass content on flexural properties of MPC at different curing times. Results illustrated that MPC flexural strength was first increased and then decreased, and 3% is the critical value for OSP mass content. Similarly, the stiffness of all specimens presented a tendency to increase first and then decrease, with a maximum value of 36.18 kN/mm appearing at 3%, i.e., the critical OSP mass content. Finally, scanning electron microscope (SEM) and X-ray diffraction (XRD) were employed to analyze the microstructure and composition of specimens, confirming that the specimens generated not only the hydration product potassium phosphate magnesium (MgKPO As a new type of inorganic cementitious material, magnesium phosphate cement (MPC) is manufactured by first mixing magnesium oxide, potassium dihydrogen phosphate, fly ash, and borax proportionally and then reacting the mixture with water ,2. BecauOyster shell powder (OSP) is a green, environmentally friendly, and renewable powdered solid, of high absorption and durability, which is produced by grinding the raw material of oyster shell after sterilization at room temperature, and which contains about 95% calcium carbonate . PreviouA total of 45 specimens with a size of 40 mm × 40 mm × 160 mm in this TPBT test were divided into 15 sets in reference to GB/T 17671-1999 , as show2PO4), borax, and fly ash (FA) in a certain proportion was poured into a cement slurry mixer and then stirred after tap water was added to produce a uniform slurry. Then, magnesium oxide (MgO) and a certain amount of OSP substituting for MgO were added into the mixer and stirred at low speed for 30 s and then at high speed for 90 s until the MPC slurry thoroughly interacted. Next, the mixed MPC slurry was poured into the mold for a complete solidification (after about 30–60 min); specimens were thus developed and demolded. Finally, all specimens were ready after being naturally cured to their corresponding time. It should be noticed that all specimens must be polished and sprayed with white paint on the outer surface to facilitate the observation of failure process before the bending test.The preparation of the OSP–MPC specimen is shown in In reference to the standard ASTM-C1609 , specimeAs the test initiated, first, a preload at a speed of 2.0 mm/min based on the displacement of the universal testing machine was added to the machine until it reached 0.02 kN, and then data began to be recorded. While the specimen remained under load at a speed of 1.0 mm/min, its load-displacement curve was recorded by a load-bearing sensor and its failure process was recorded by a high-definition camera during the bending test. The test was terminated when specimen’s residual load reached 10% of the peak load. In addition, some failed specimens were used for SEM, EDX, and XRD tests to observe specimens’ microstructures and hydration products under different dosages of OSP, so as to facilitate the interpretation of the observations in the bending test.XRD was applied to analyze sample elements and compound content changes. The basic process for results of X-ray diffraction effects on materials uses sample atoms to show the primary microscopic ion excitation, i.e., X-ray photons produce secondary X-ray and X-ray diffraction patterns. We used Jade software after analyzing the diffraction patterns and sample composition spectrum diffraction peaks. Preparation of XRD samples: the samples are ground into powder by ball mill, the powder is ground through 200 target screening, to achieve the fineness of the test sample, sealed and preserved; XRD test process: fill the central groove of the glass slide with OSP powder; use cover glass to smooth the protrusion of powder; use a small brush to clean the residual powder at the edge of the groove; put into X-ray diffraction chamber for 5°~80° wide angle test.2/kg, density of 2650 kg/m3, and particle size of 45 μm. Detailed chemical composition is listed in The mixing proportion of all specimens shown in The oyster shell powder used in this project was obtained by grinding discarded oyster shells into powder. Its XRD analysis is shown in For specimens in Group T7 with no OSP (Group OSP0-T7), typical brittle failure emerged. Shortly after loading, tiny splits appeared in the center bottom of the specimen, with no obvious failure. Then, the splits rapidly stretched across the specimen, bringing about a crisp cracking sound within seconds and a brittle failure with two parts still attached to each other. Brittle failure showed up when OSP was incorporated and grew more apparent as OSP mass content increased. For example, as shown in With the same OSP mass content, specimens in Group T14 and T28 presented a similar failure process to that of Group T7. Specimens in Group T14 did not break into two parts when they were loaded to their limit, and their width of the mid-span crack at the bottom section was less than that of the specimen with no OSP. As for the specimens in Group T28, when the ultimate load was added, the width of the mid-span crack at the bottom section was more overt than that in the Group T7 and T14. In addition, the cross-interruption surface of the specimen after its failure was intercepted as shown in As mentioned earlier, specimens in Group T7 increased their loading load to the peak point (point A) in an approximately linear way, and then dropped it sharply to point B. The peak displacement and secant stiffness of specimens are shown in Specimens in Group T14 and T28 displayed a similar trend in L-D curves to that of Group T7, but differed in Ks, i.e., for a longer curing time, the Ks of specimens at OSP mass content ranging from 6% to 12% decreased less than that of 0% of OSP mass content. Taking Group T28 as an example, when OSP mass content increased from 6% (M-SW6-T28) to 12% (M-SW12-T28), secant stiffness decreased by 25.7%, 46.2%, and 53.2%, respectively compared to 0% of OSP mass content (M-SW0-T28). However, for Group T7, compared to OSP mass content of 0% (M-SW0-T7), secant stiffness reduced by 30.4%, 46.7%, and 55.2%, respectively as OSP mass content increased from 6% (M-SW6-T7) to 12% (M-SW12-T7). In addition, curing time similarly affected the relationship between peak displacement and OSP mass content. On the contrary, the gap in secant stiffness between specimens in Group T7 and Group T14 decreased with the prolonging of curing time, as shown in fR is the flexural strength, uP is the peak load, L is the supporting distance (100 mm), b is the width of specimen (40 mm), and h is the height of specimen (40 mm).The flexural strength of a specimen is calculated using formula (1) according to ASTM C293 , and finFor specimens in Group T14 and T28, OSP mass content had a similar effect on their flexural strength. Flexural strength rose as OSP mass content increased to 3%, and then dropped as OSP mass content continued its augmenting. Therefore, it can be concluded that 3% of OSP is the most appropriate dosage to improve MPC bending performance, while excessive OSP would impair it. This might be due to the decreasing amount of cementitious materials. When OSP mass content was unchanged, its flexural strength increased significantly with the extension of curing time. In addition, no regularity was found in the influence of curing time on the compressive strength with the increase of OSP mass content.SEM was used to study the influence of OSP mass content on the microstructure of MPC. The SEM sample preparation process causes errors which affect the SEM images ; after s3, the main component of OSP, CaHPO4·2H2O was detected after the incorporation of OSP, with OSP mass content increasing from 3% to 12% and its maximum intensity dropping from 1318 a.u. to 599 a.u. This phenomenon may be ascribed to two reasons. The first reason is the hydration of MPC [2PO4 was dissolved into potassium ion and dihydrogen phosphate ion, and MgO was converted into hydroxyl ions (OH−) and magnesium ions (Mg2+) through the interaction of free water, therefore MKP was generated by Mg2+ finally interacting with K+, PO43− and bound water from H+ and OH−, as shown in 2+) were dissolved from CaCO3 in OSP under the assistance of free water, as shown in the figure, and then reacted through combining with the remaining phosphate ions (PO43−) in the matrix to produce CaHPO4, as shown in 4 could fill in the internal pores and enhance the matrix strength. Matrix density was also well promoted through the interaction of hydration products MKP and CaHPO4, as shown in 4·2H2O, finally degrading the matrix strength. In the comparison of Group T7 with Group T14, their variation trends were similar to that of T28 group, and it was discovered that the diffraction peak intensity of MKP and CaHPO4·2H2O gradually increased as the curing time increased. Therefore, specimens in Group T28 exhibited the highest flexural strength.In order to further analyze the composition of the filling material inside the MPC pores after adding OSP, XRD analysis was carried out. n of MPC ,26. KH2P(1)Limestone has similar compositions and properties to OSP, and the strength of MPC can be slightly increased by partially replacing magnesia in MPC with 5% limestone, while the strength of MPC decreases as the limestone content continues to increase . In this(2)OSP mass content has an identical effect on the bending properties of MPC at different curing times. However, specimens at 28 curing days exhibit greater flexural strength and higher stiffness than those at 7 days and 14 days.(3)OSP can improve the bending strength to a certain extent, which is however confined by its mass content. When OSP mass content is greater than 3% (in this study), flexural strength will decrease. Further research is needed to obtain a more accurate critical value for OSP mass content.(4)SEM analysis proves that as curing time increases, the development of specimens is relatively complete, the rod-like crystal structure gradually weakens, and the network structure gradually becomes dense. As a result, the strength of specimen gradually increases.(5)4·2H2O) is also generated, and pore structure in the matrix is optimized to interact with MKP, which mutually improve the mechanical properties of MPC.XRD analysis demonstrates that in addition to the main hydration product struvite and the residual magnesium oxide, a new reactant (CaHPOIn this study, a typical three-point bending test was employed to discover the influence of OSP mass content on the failure mode, flexural strength, and deflection behavior of MPC under different curing times. In addition, analysis techniques of SEM and XRD were adopted to study the new reaction products and morphology of OSP–MPC cement paste. In view of the results, the following conclusions can be drawn:


Bagnat, MichelKumar, ManuBakht, MartinLewsey, Mathew G.Cava, ClaudiaLiss, Andrew S.Chen, Pao-YangLomberk, GwenCheng, Yuen YeeLunardon, AliceChüeh, Anderly C.Maleszka, RyszardCorces, VictorMione, MarinaCrisp, PeterMoin, MazaharDe La Serna, IvanaMuchardt, ChristianDi Pizio, AntonellaNandi, SaikatDoni Jayavelu, NareshNestor, Colm E.Elliott, HannahOlova, NellyEl-Rifai, WaelPérez-Lluch, SílviaFu, BeidePerucho, ManuelFuso, AndreaRoccaro, AldoGao, LongRönn, TinaGood, Deborah J.Satyaki, P.R.V.Gradziel, Thomas M.Saze, HidetoshiGuan, XueyingSchweiger, Michal R.Harris, R. AlanShen, Che-Kun JamesHassan, QuamarulToh, Tan BoonHernandez-Vargas, HectorTrollope, AlexandraHo, Eric S.Tucci, ValterHuang, JijunUlicna, LiviaIlmer, MatthiasVan Ness, BrianIm, Chang-NimVarotto, SerenaJha, SudhakarVélez-Cruz, RenierJHANWAR, SHALUVerde, GaetanoJin, PengWang, Bang-AnJung, Chol-HeeZaidi, Syed Shan-e-AliKandimalla, RajuZapico, Sara C.Kast, Richard EricZhu, JianKleeff, JörgZhu, Jian-KangKnapp, StefanZhu, Qian-HaoKramer, Jamie M.Rigorous peer-review is the corner-stone of high-quality academic publishing. The editorial team greatly appreciates the reviewers who contributed their knowledge and expertise to the journal’s editorial process over the past 12 months. In 2018, a total of 21 papers were published in the journal, with a median time to first decision of 15 days and a median time to publication of 38 days. The editors would like to express their sincere gratitude to the following reviewers for their cooperation and dedication in 2018:


Coronally advanced flap (CAF) by tunneling procedure was applied on four cases of gingival recession. Post‐operative follow‐up, at different time breaks, recorded full coverage of almost all receded root surfaces. The technique and the clinical outcome of this technique will be demonstrated in this case series report. Coronally advanced flap (CAF) by tunneling procedure is considered one of the effective root coverage procedures, particularly when it is combined with CTG, in modification of the conventional technique. Post‐operative follow up, at different time breaks, recorded full coverage of almost all receded root surfaces. Details of the surgery and the possible complications were explained to the patients, and signed informed consent was taken from them before starting the surgical procedures. Further, the study proposal was submitted to the scientific committee of the college of dentistry, University of Sulaimani, for registration and obtaining ethical approval for undertaking this study.3Root surface debridement was performed with a curette after giving local anesthetics to the area by infiltration. Tunneling was performed using a Hu‐friedy tunneling knife (TKN1 #1 HDL #6) and a fine tissue separator (Dentag Evo) Figure . AccordiThe graft was placed under the tunnel and sutured from either side. In the current study, the graft was retained by either 2 circular stitches around adjacent teeth or with composite filling. This was done to hold part of the graft fixed over the receded roots and the other part over the underlying bone, without being sutured to the flap, to retain the graft fixed in place and avoid dislodgment under possible tension. In multiple recession cases, the flap margin was sutured independently and fixed by composite filling to the facial surfaces of teeth Figure .4The study included 3 cases, 2 of which were single gingival recession (RT2), Figures 5The incision free design and gingival papillary preservation are considered as the main advantages of TUN.In these cases, the flap was further extended on both sides and the apical side to provide a relaxed bed for the graft. Therefore, this method of tissue preparation and CTG suturing may provide high stability of the graft in terms of mechanical and biological aspects. In this procedure, the CTG is completely secured by stretching it laterally and suturing around the teeth adjacent to the recession on both sides without suturing to the underlying periosteum and/or overlying flap tissue. Stretching the graft avoids shrinkage and improves the survival rate by making the graft more responsive to revascularization.Higher predictability rate of the clinical outcome could be expected with the current procedure, while the tunnel flap and the graft are relaxed and not under tension to avoid any mobility of the graft that compromises the normal healing process.6With limited number of cases presented in this manuscript, the tunneling procedure for root coverage showed high predictable positive outcomes.No conflict of interest was declared by the authors of this study.DK involved in design and case documentation. FZ involved in manuscript preparation and final approval of the manuscript.Written informed consent was obtained from the patient to publish this report in accordance with the journal's patient consent policy.