Simultaneous Qualitative and Quantitative Study of Main Compounds in Commelina communis Linn. by UHPLC-Q-TOF-MS-MS and HPLC-ESI-MS-MS.
This study reported the identification and determination of the main components of Commelina communis Linn. A total of 62 compounds were identified in C. communis Linn. extract, which included 29 flavonoids and flavonoid glycosides, 17 phenolic acids, 4 alkaloids, 1 pyrimidine alkaloids, 3 sterols and 8 fatty acids and others by ultra high performance liquid chromatography coupled with hybrid triple quadrupole time-of-flight mass spectrometry. Moreover, a specific, simple, rapid and sensitive high performance liquid chromatography with tandem mass spectrometry method was developed and validated for determination of 13 components of C. communis Linn., which included orientin, iso-orientin, vitexin, isovitexin, rutin, apigenin, protocatechuate, vanillic acid, caffeic acid, ferulic acid, luteolin, quercetin and isorhamnetin. All calibration curves showed good linearity (r ≥ 0.9991) within the test range. The intra- and inter-day precisions (relative standard deviation%, RSD%) were within 1.04 and 0.92%, and the recoveries ranged from 98.64 to 100.8%. These results may contribute to the further study and quality control for C. communis Linn.
UPLC-Q-TOF-MS Study of the Mechanism of THSWD for Breast Cancer Treatment
Taohong Siwu decoction (THSWD) is a classic traditional Chinese medicine (TCM) prescription that is widely used in the clinical treatment of gynecological and cerebrovascular diseases. Here we used a method that coupled ultra-performance liquid chromatography to quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) in which both positive and negative ion modes were established to investigate the major constituents in THSWD. A Waters ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm) was used to separate the aqueous extract of THSWD. The mobile phase consisted of 0.1% aqueous formic acid (A) and acetonitrile (B). Ninety-five components were identified in two different ion modes, including aromatic acids, flavones, polysaccharides, volatile oils monoterpene glycosides, aromatic cyanogenic glycosides, and others. Pathological changes in tumors and serum expression of interleukin-4 in a mouse model of breast cancer were detected after THSWD treatment. The results showed that THSWD had obvious therapeutic effects. This study establishes a material basis for the use of THSWD in the treatment of breast cancer.
Mass defect profiles of biological matrices and the general applicability of mass defect filtering for metabolite detection.
Recent examples have demonstrated that the high-resolution liquid chromatography/mass spectrometry (LC/MS)-based mass defect filtering (MDF) technique was effective in selectively detecting drug metabolites regardless of their molecular weights or fragmentation patterns. The main objective of the current study was to evaluate the general applicability of MDF for drug metabolite detection in typical biological matrices. Mass defect profiles of commonly used biological matrices including plasma, urine, bile, and feces were obtained using an LTQ FT mass spectrometer and were compared with those of 115 commonly prescribed drugs. The mass defect profiles were presented as two-dimensional Y-X plots with the determined mass defects of components on the y-axis versus the corresponding m/z values on the x-axis. The mass defect profiles of the matrices appeared to be similar for each type of matrix across species, yet marked differences were apparent between matrices of a given species. The mass defect profiles of components in plasma, bile, and feces showed significant separation from most of the 115 drugs. The mass defect profiles of urine did not show such clean separation from that of the 115 drugs. The results suggest that MDF has a broad applicability for selective detection of drug metabolites in plasma, bile and feces although the selectivity for detecting urinary drug metabolites is not as good as in the other matrices. In addition, the mass defect profiles of the biological matrices allow for prediction of the effectiveness of MDF for certain applications, and for designing specific MDF windows for selective detection of drug metabolites.