Simultaneous determination of four sesame lignans and conversion in Monascus aged vinegar using HPLC method.
A simple, accurate and specific high-performance liquid chromatography (HPLC) method has been developed and validated for simultaneous determination of sesamol, sesamin, asarinin and sesamolin in Monascus aged vinegar. The effects of acid hydrolysis and four heating treatments on the components content in Monascus aged vinegar were discussed. The results showed that the isomerisation of sesamin to asarinin, and decomposition of sesamolin to sesamol significantly increased, regardless of heating or acid hydrolysis. Thermal processes and acid hydrolysis increased the content of sesamol and asarinin, respectively, but severe thermal processes resulted in the loss of total sesame lignans. Sesamol and asarinin reached the highest (2.720 ± 0.202 μg/mL and 2.064 ± 0.075 μg/mL) for autoclaving (125 °C, 15 min) and acid hydrolysis (25 °C, 15 min, nature pH), respectively. Therefore, autoclaving and acid hydrolysis were considered as the optimal way to obtain higher content of sesamol and asarinin.
The epimerization of sesamin and asarinin.
Sesamin (1) and asarinin (2) are two C-7' epimeric lignans. Molecular modeling by semiempirical methods indicated that 1 is more stable than 2 by about 2.5 kcal/mol. However, epimerization under acidic conditions led to a 44.8/55.2 equilibrium ratio of 1 and 2. Single-crystal X-ray diffraction analyses indicated that 1 was monoclinic with a = 10.0435(19) A, b = 6.9151(8) A, c = 11.8460(13) A, and 2 was triclinic with a = 5.595(5) A, b = 9.5910(18) A, c = 15.620(4) A. The unexpected equilibrium ratio of 1 and 2 indicated that structural changes are dependent on the conditions of the extraction processes.
Evaluation of Analgesic Effect of Caudal Epidural Tramadol, Tramadol-Lidocaine, and Lidocaine in Water Buffalo Calves (Bubalus bubalis)
Aim of this study was to compare the analgesic effect of tramadol and a combination of tramadol-lidocaine with that produced by lidocaine administration in the epidural space in buffalo calves. In a prospective randomized crossover study, ten male buffalo calves were used to compare the epidural analgesic effect of tramadol (1 mg/kg) and tramadol-lidocaine combination (0.5 mg/kg and 0.11 mg/kg, resp.) with that produced by 2% lidocaine (0.22 mg/kg). Loss of sensation was examined by pin-prick test. Onset time, duration, and degree of analgesia and ataxia were recorded after each treatment. Heart rate (HR), respiratory rate (RR), rectal temperature, and haematobiochemical parameters were recorded after all treatments. Time to onset and duration of analgesia, respectively, were as follows: tramadol 11 ± 2 min and 208 ± 15 min; tramadol-lidocaine 6 ± 2 min and 168 ± 9 min; lidocaine 4 ± 1 min and 67 ± 13 min. Onset time and duration were significantly longer with tramadol than the other treatments. Duration was significantly longer with tramadol-lidocaine than lidocaine. Ataxia was mildly observed in tramadol-lidocaine and was moderate in lidocaine. HR, RR, and rectal temperature did not differ significantly from baseline after any treatment. Haematobiochemical parameters returned to basal levels by 24 h after all treatments. This combination might be clinically useful to provide analgesia in buffalo for long-duration surgical procedures.