Résumé
Objective: To establish a rapid qualitative analysis method for fatty acids and esters in Coicis Semen by ultra-performance liquid chromatography triple quadrupole time-of-flight mass spectrometry (UPLC-Triple-TOF-MS). Methods: Agilent ZORBAX-SB C18 (250 mm × 4.6 mm, 5.0 μm) column was used. The mobile phase was acetonitrile-isopropanol (1:1) elution, the flow rate was 1 mL/min, the detection wavelength was 210 nm, the column temperature was 30 ℃, and the injection quantity was 10 μL. Electrospray ion source positive ion mode was adopted, and the scanning range was m/z 100-1 500. The sample data were collected by full scanning mode, and the fatty acid chemical composition of Coicis Semen was quickly identified according to the information obtained by high-resolution mass spectrometry combined with secondary mass spectrometry. Results: A total of 29 kinds of fatty acids and esters in Coicis Semen were detected, and the cracking rules of the compounds were analyzed. Through the mass-to-charge ratio of molecular ion peaks and fragment ions, the Scifinder and Reaxy network databases, and the literature, these compounds were different under the action of ion source by losing the structure of oleic acid, linoleic acid, palmitic acid, oxidizing oleic acid and the like. The mass-to-charge ratio of the fragment ions, and the name and structural formula of the 29 fatty acids and their ester compounds were inferred. Conclusion: The method of qualitative analysis of the fatty acids and esters of Coicis Semen established in this study is accurate, rapid and sensitive, which provides experimental basis for improving the quality control level of Coicis Semen and further elucidating the pharmacodynamic substance basis of Coicis Semen.
Résumé
Objective: To establish a quick method of ultra-performance liquid chromatography-quadrupole time-of-fight mass spectrometry (UPLC-Triple-TOF/MS) for the analysis of compounds in Tetrastigma hemsleyanum. Methods: The separation was performed on the chromatographic column of Agilent Eclipse Plus-C18 (100 mm × 4.6 mm, 1.8 μm), and the mobile phase was methanol (0.1% formic acid)-0.1% formic acid solution, with a gradient elution at a flow rate of 1 mL/min. The column temperature was 30℃, and negative ion mode was used for TOF-MS. Results: Fifty-one compounds were identified or tentatively characterized based on the retention time and MS spectra. They are flavonoids, phenolic acids, phospholipids, glycolipids, benzenesulfoic acid, etc. And the preliminary fragmentation rules of phospholipid, glycolipids, and benzenesulfoic acid were summarized. Conclusion: The results demonstrate that UPLC-Triple-TOF/MS method is novel, quick, and efficient for the identification of the compounds in T. hemsleyanum.
Résumé
Objective: To analyze the change of chemical constituents of Polygoni Multifori Radix from different harvest time. Methods: Fifteen batches of Polygoni Multifori Radix samples from different harvest time were determined by UPLC-Triple TOF-MS/MS. Through the analysis of the multistage tandem mass spectrometry, the characteristic peaks were extracted with mass spectrometry data peak matching, peak alignment, and noise filtering. Principal component analysis (PCA) and partial least-squares discriminant analysis (PLS-DA) were used for data processing. The components were identified according to a mass spectrometry accurate mass and two mass spectrometry fragmentation information, combined with the software of database search and literature. Results: The chemical composition in Polygoni Multifori Radix samples from different harvest time are clearly distinguished. Twenty-four kinds of differential chemical constituents were identified. Among them, there are nine kinds of common differential constituents which presented different changing laws. Conclusion: This study provides the basic data for revealing the dynamic change law of metabolite accumulation of Polygoni Multifori Radix and confirms its optimal harvest period.
Résumé
Objective: To analyze the difference of chemical compositions in Xanthii Herba and Xanthii Fructus. Methods: Eight batches of Xanthii Herba and Xanthii Fructus samples from different origins were determined by UPLC-Triple TOF-MS/MS. Through the analysis of the multistage tandem mass spectrometry, the characteristic peaks were extracted with mass spectrometry data peak matching, peak alignment, and noise filtering. Principal component analysis (PCA) and partial least-squares discriminant analysis (PLS-DA) were used for data processing. The components were identified according to a mass spectrometry accurate mass and two mass spectrometry fragmentation information, combined with the software of database search and literature. Results: The chemical compositions in Xanthii Herba and Xanthii Fructus samples are clearly distinguished. Forty-four compositions have the differences between Xanthii Herba and Xanthii Fructus. Forty-one chemical compositions are identified. Among of them, there are 12 kinds of differential compositions which presented different changing laws. Conclusion: From the different compositions of Xanthii Herba and Xanthii Fructus, the material basis can be provided for revealing the property and efficacy in Xanthii Herba and Xanthii Fructus.
Résumé
OBJECTIVE: To analyze the differences in chemical composition of Pseudostellariae Radix from different germplasms. METHODS: Tweny-four batches of samples were determined by UPLC-Triple TOF-MS/MS. Characteristic peaks were extracted through treatment of mass spectrometry data including peak matching, peak alignment and noise filtering. Principal component analysis (PCA) and partial least-squares discriminant analysis (PLS-DA) were used for data processing. Component identification was carried out based on the mass spectrometry accurate mass and secondary mass spectrometry fragmentation information combined with database search and literature. RESULTS: The differences among samples of Pseudostellariae Radix of different germplasms were distinguishable. Twenty-one chemical compositions with significant differences were screened, among which 10 common chemical compositions showed different changing laws. CONCLUSION: This study provides experimental data for revealing the laws of Pseudostellariae Radix metabolites from different germplasms.
Résumé
Objective: To analyze the changes of chemical composition of Pseudostellariae Radix using different processing methods. Methods: To determine 20 batches of samples by UPLC-Triple TOF-MS/MS and tandem mass spectrometry and by combining Mass data, database, and related software for total ion current literature major molecular ion peaks attributable. Data processing was carried out using SIMCA-P software to study multivariate statistical analysis. Results: Thirteen compounds were identified, and the differences of PCA between samples of Pseudostellariae Radix using different processing methods were distinguishable, and 11 kinds of markers were picked from loading chart by significant differences. The 11 kinds of markers presented different changing laws. Conclusion: The research provides experimental data for revealing the laws of different processing methods on metabolites of Pseudostellariae Radix.