Identification of Chemical Constituents in Chaishi Tuire Granules by UPLC-ESI-Q-TOF-MS/MS / 中国实验方剂学杂志

Objective:To rapidly identify the chemical constituents of Chaishi Tuire granules by ultra-performance liquid chromatography-electrospray/quadrupole time-of-flight tandem mass spectrometry （UPLC-ESI-Q-TOF-MS/MS）. Method:Chromatographic separation was conducted on a Phenomenex^® Luna omega C₁₈ column （2.1 mm×100 mm， 1.6 μm） with 0.1% formic acid aqueous solution （A）-acetonitrile （B） as the mobile phases for gradient elution （0-20 min， 5%-40%B； 20-40 min， 40%-95%B； 40-43 min， 95%B）， the flow rate was set at 0.3 mL·min^-1. MS data were collected in positive and negative ion modes， the scanning range was <italic>m</italic>/<italic>z</italic> 150-1 500 and electrospray ionization （ESI） was employed. The chemical constituents of Chaishi Tuire granules were identified by comparing with the retention time and the mass data of the reference substances， as well as the accurate mass， MS/MS fragment ions， mass spectrometry databases （PubChem， MassBank， ChemicalBook and others） and related literature. Result:A total of 85 chemical constituents were identified， including 28 flavonoids， 24 phenylpropanoids， 11 terpenoids， 10 alkaloids， 4 quinones， and 8 others. Among them， 19 constituents derived from Lonicerae Japonicae Flos， 14 constituents derived from Scutellariae Radix， 10 constituents derived from Isatidis Radix， 9 constituents derived from Taraxaci Herba， 9 constituents derived from Forsythiae Fructus， 4 constituents derived from Bupleuri Radix， 4 constituents derived from Anemarrhenae Rhizoma， and 4 constituents derived from Rhei Radix et Rhizoma. Conclusion:Chaishi Tuire granules is rich in phytochemicals， which are derived from many of traditional Chinese medicines. This study can lay a foundation for the quality control， material basis and <italic>in vivo</italic> metabolic analysis of this preparation.

Chemical constituents of Shuangshen Pingfei Granules by UPLC-ESI-Q-TOF-MS/MS / 中草药

Objective: A novel ultra-performance liquid chromatography tandem quadrupole time of flight mass spectrometry (UPLC-Q-TOF-MS/MS) was applied to establish a method to recognize and classify the main chemical constituents of Shuangshen Pingfei Granules accurately and rapidly. Methods: ACQUITY UPLC® BEH C18 chromatographic column (100 mm × 2.1 mm, 1.7 μm) was employed to UPLC analysis with the mobile phase consisting of acetonitrile-0.1% formic acid aqueous solution. ESI ion source was used to ensure the data collected in positive and negative ion mode. The chemical components of Shuangshen Pingfei Granules were identified by comparing with the retention time and the mass data of the reference substance, and consulting literature reports and mass spectrometry database. Results: A total of 63 chemical components were identified, including 24 terpenoids, seven phenolic acids, six tanshinones, 14 flavonoids and 12 other classes. Conclusion: The qualitative method established in this study could be used to rapidly and accurately identify the main chemical constituents of Shuangshen Pingfei Granules, and lay a foundation for the further analysis of effective ingredients in vivo, pharmacodynamic material basis and quality control research.

Chemical constituent analysis for seeds of Celosia argentea by UPLC-ESI-Q-TOF-MS / 中国中药杂志

This Paper aimed to analyze and identify the chemical constituents from the seeds of Celosia argentea by UPLC-ESI-Q-TOF-MS. The analysis was performed on an ACQUITY HSS T3 reverse phase column(2.1 mm ×100 mm, 1.8 μm). The mobile phase consisting of 0.1% formic acid acetonitrile and 0.1% aqueous formic acid was used for gradient elution, and the flow rate was 0.4 mL·min~(-1). Mass spectrometry was applied for the qualitative analysis under positive and negative ionization modes and ESI ion source. Data was analyzed by Masslynx 4.1 software, literatures in SciFinder database, and standards. A total of 49 compounds, including 14 triterpenoids, 17 flavonoids, 11 cyclic peptides, 2 phenols, 2 organic acids, and 3 steroids were putatively identified. Among them, 19 compounds were firstly reported from this species. In-depth chemical constituent analysis for the seeds of C. argentea were accomplished here, and the findings could lay a good foundation for its quality control and clarifying the material basis of its efficacy.

Rapid identification of constituents of Urtica hyperborea using UPLC-ESI-Q-TOF-MS/MS method / 中国中药杂志

This paper deals with the application of ultra-performance liquid chromatography tandem quadrupole time of flight mass spectrometry(UPLC-ESI-Q-TOF-MS/MS) method to rapidly determine and analyze the chemical constituents of methanol extract of Urtica hyperborea. We employed UPLC YMC-Triart C18(2. 1 mm×100 mm,1. 9 μm) column to UPLC analysis with acetonitrile-water(containing 0. 4% formic acid) in gradient as mobile phase. The flow rate was 0. 3 m L·min-1 gradient elution and column temperature was 30℃; the injection volume was 4 μL. ESI ion source was used to ensure the data collected in anegative ion mode. The chemical components of U. hyperborea were identified through retention time,exact relative molecular mass,cleavage fragments of MS/MS and reported data.The results indicated that a total of 31 compounds were identified,including 8 flavonoids,14 phenolic compounds,8 phenylpropanoids(4 coumarins and 4 lignans),and 1 steroidal compound,13 of which were confirmed by comparison. The UPLC-ESI-Q-TOF-MS/MS method could rapid identify the chemical components of U. hyperborea. The above compounds were discovered in U. hyperborea for the first time,which could provide theoretical foundation for further research on the basis of the pharmacodynamics of U. hyperborea.

Analysis on chemical constituents from Swertia mileensis by UPLC-ESI-Q-TOF-MS / 中草药

Objective: To analyze and identify the chemical constituents from Swertia mileensis by UPLC-ESI-Q-TOF-MS. Methods: The analysis was performed on an Acquity HSS T3 reverse phase column (100 mm × 2.1 mm, 1.8 μm). The mobile phase consisted of 0.1% formic acid acetonitrile and 0.1% formic acid, and was used for gradient elution, with the flow rate of 0.4 mL/min. Mass spectrometry was applied for the qualitative analysis under positive and negative ion modes and ESI ion source. Data was analyzed by Masslynx 4.1 software, SciFinder database, literatures, and standards. Results: Twenty-eight compounds, including 7 iridoids, 14 xanthones, 3 flavonoids, 2 triterpenes, and 2 phenols were identified from S. mileensis. Among them, vogeloside, 8-O-β-D- glueopyranosyl-(l→6)-β-D-glueopyranosyl-l,7-dihydroxy-3-ethoxyxanthone, 3-O-demethylswertipunicoside, and sweriyunnanlactone A were reported from this species for the first time. Conclusion: Using UPLC-ESI-Q-TOF-MS method the main chemical constituents from S. mileensis can be rapidly and accurately identified, which provides a new strategy for its quality control as well as a reference for clarifying the material basis of its efficacy.

Chemical constituents from water extract of Toosendan Fructus by UPLC-ESI-Q-TOF-MS / 中草药

Objective: To analyze and identify the chemical constituents from the water extract of Toosendan Fructus by UPLC-ESI- Q-TOF-MS. The analysis was performed on an ACQUITY HSS T3 reverse phase column (2.1 mm × 100 mm, 1.8 μm). The mobile phase consisted of acetonitrile and 0.1% formic acid was used for gradient elution, the flow rate was 0.4 mL/min. Methods: Quadrupole-time of flight-mass spectrometry was applied for the qualitative analysis under positive and negative ion modes and ESI ion source was used for mass spectra. Results: The results indicated that fifteen compounds from the water extract of Toosendan Fructus had been identified by direct comparison in both positive and negative ion mass data, the element compositions analysis, and the data of the literature. They are vanillic acid, lilac acid, p-hydroxybenzoic acid, rutin, meliatoosenin E, toosendanin, Δ5,6-isotoosendanin, isotoosendanin, meliatoosenin N, meliatoosenin P, 1-deacetylnimbolinin B, meliatoosenin R, 1-O-tigloyl-1-O-debenzoylohchinal, meliatoosenin R, and nimbolinin B. Conclusion: The efficient separation ability of UPLC and high sensitive detection of MS are used in this study, which will provide the evidences for evaluating the quality of Toosendan Fructus herbs, stabilizing the curative effect in clinic, and explaining the mechanism.