ABSTRACT
Objective: To study the chemical differences between natural and synthetic of Bambusae Concretio Silicea by ultra-high performance liquid chromatography-quadrupole tandem time-of-flight mass spectrometry (UPLC-Q-TOF-MS). Methods: The qualitative analysis of chemical composition was made combined online database and secondary fragmentation cleavage rules, and difference analysis was carried out by the Enhance Peak Find function of PeakView software. Then the converted data was imported into SIMCA-P software to establish an OPLS-DA statistical model and differential secondary metabolites were analyzed. Results: The constituents of Bambusae Concretio Silicea mainly included amino acids, organic acids, alkaloids, glycosides, etc. Among them, 11 components were known, while other 43 compounds were identified for the first time. A total of 14 distinct components, including 2,5-dimethyl-1,3-oxazole-4-carboxylic acid and sucrose, and 12 biomarkers, including 4-(heptyloxy)phenyl-4-(hexyloxy)benzoate, and N-lauryldiethanolamine were identified. Conclusion: This study reveals that the chemical differences between the two herbs are obvious, while betaine and sucrose can be used as the distinguishing indicators. And it provides new ideas and data references for the quality control and clarification of medicinal substances.
ABSTRACT
OBJECTIVE: To identify the main chemical constituents in the extract of deep fried strychnas by UPLC-Q-TOF-MS. METHODS: Agilent SB-C18(2.1 mm×100 mm, 1.8 μm) column was used. Gradient elution was conducted with mobile phase consisting of 0.1% formic acid solution (A) and acetonitrile (B)at a flow rate of 0.2 mL•min-1. The column temperature was maitained at 35 ℃. MS analysis was based on information associated mode (IDA) that positive and negative ions were respectively collected. RESULTS: A total of 31 compounds were identified in deep fried strychnas, of which eight had not been reported as Semen Strychni,and four new compounds were found in the positive and negative ion mode. The main chemical constituents included alkaloids, organic acids, glycosides, etc. CONCLUSION: The method is accurate, reliable, and efficient, and is suitable for rapid identification of the ingredients in deep fried strychnas, which provides a reference for the development and utilization of processed products of Semen Strychni and clarification of its efficacy and material basis.
ABSTRACT
Objective: To establish UPLC-Q/TOF method for simultaneous qualitative and quantitative analysis of main chemical components in Sinodielsia yunnanensis. Methods: High performance liquid chromatography tandem flight time mass spectrometry was used. Chromatographic column was Agilent shell 120 Hilic, and the flow phase was acetonitrile-0.1% acid aqueous solution (gradient elution) at a flow rate of 0.3 mL/min; Qualitative and quantitative analysis adopted Q-TOF positive anion full scanning + IDA (information correlation acquisition) mode. Results: Using the established screening database, the target compounds with a mass error of less than 5×10-6, a correct isotope distribution and fragment ion are used as the target compounds. Combined with software Formula Finder, Mass Calculators and other functions, online database (Human Metabolome Database, PubChem, Chemical Book, etc.), and two stage fragmentation rule, 23 compounds were identified by qualitative identification. Ferulic acid was determined as a quantitative indicator component, and the quantitative and qualitative ions were 178 and 149, respectively; The linear range was 1.14-1 140 ng/mL (r = 1.000), and the limits of detection and quantitation respectively was 0.87 ng/mL and 2.91 ng/mL; RSDs of precision, stability, and reproducibility tests were lower than 2%; The recovery rate was 98.13%-101.25% (RSD = 1.37%, n = 5). Conclusion: This method has high sensitivity, good reproducibility, and its analysis is fast, accurate, and reliable, and it can be used for simultaneous qualitative and quantitative determination of main chemical components in the medicinal materials of S. yunnanensis; The content of ferulic acid in Yunnan is higher than that in Tibet.
ABSTRACT
Caffeine and its metabolic products play an important role in clinical applications. An ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF MS/MS) method was applied to systemically study the caffeine metabolism in liver microsomes of rats and mice, and comprehensively evaluate caffeine metabolites in vitro and metabolism differences between species. The caffeine metabolites and metabolism differences between species in liver microsomes of rats and mice were analyzed by UPLC-Q-TOF-MS/MS high resolution mass spectrometry system and metabolitepolite software. The results showed that in addition to the demethylated and oxidized products in previous analysis, methylated, double oxidized, dehydrated and decarbonylated metabolites were also found in caffeine metabolism in liver microsomes of rats and mice, with significant difference in metabolism in vitro between rats and mice. The demethylated metabolite M2(C7H8N4O2) and decarbonylated metabolite M6(C7H10N4) in metabolism in vitro of mice were not found in rats, and the in vitro metabolite M7(C8H12N4O5) in rats were not found in mice. There was significant species difference in caffeine metabolism in vitro between rats and mice, providing important reference value for the further metabolism study and safety evaluation of caffeine.