UPLC-Q-TOF-MS/MS和GC-MS法分析银翘清热片化学成分

Analysis of Chemical Components of Yin-Qiao-Qing-Re Tablets by UPLC-Q-TOF-MS/MS and GC-MS

    摘要
  • 摘要:
    目的 采用超高效液相色谱串联四极杆飞行时间质谱联用技术(UPLC-Q-TOF-MS/MS)和气相色谱-质谱联用仪技术(GC-MS)分别分析银翘清热片中非挥发性和挥发性化学成分。
    方法 非挥发性成分采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm，1.7 μm)，流动相为0.1%甲酸水溶液(A)和乙腈(B)进行梯度洗脱，流速0.35 mL·min-1，进样量5 μL，柱温30 ℃；挥发性成分采用Agilent SH-I-5MS色谱柱(5%Phenyl methyl silox，30 m×250 μm，0.25 μm)，程序升温，进样量为1 μL，分流比为10 ∶ 1，流速为1.0 mL·min-1，进样口温度为200 ℃。
    结果 从银翘清热片中共分析和鉴定出134个非挥发性化学成分和23个挥发性成分，其中49个化合物经对照品比对验证。非挥发性成分主要包括27个黄酮类，21个有机酸类，15个木脂素类，14个环烯醚萜类，12个苯乙醇苷类，11个皂苷类，10个生物碱类，5个萜类，4个氨基酸类，3个苯丙素类，3个双苯吡酮类，3个核苷类，3个酚苷类，2个色原酮类和1个糖类。挥发性成分主要包括11个单萜类，5个醇酚类，3个烯类，2个酮类，1个酯类和1个烃类成分。
    结论 快速鉴定了银翘清热片的化学成分，为银翘清热片的药效物质基础研究和完善质量控制标准奠定前期基础。

     

    Abstract:
    OBJECTⅣE The non-volatile and volatile chemical components in Yin-Qiao-Qing-Re Tablets were analyzed separately using ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS) and Gas Chromatography Mass Spectrometry (GC-MS).
    METHODS The non-volatile components were analyzed using a Waters ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm), with a mobile phase consisting of 0.1% formic acid aqueous solution (A) and acetonitrile (B) for gradient elution, a flow rate of 0.35 mL ·min-1, an injection volume of 5 μL, and a column temperature of 30 ℃; the volatile components were analyzed using an Agilent SH-I-5MS column (5% Phenyl Methyl Silox, 30 m×250 μm, 0.25 μm); the procedure was temperature-programmed, with an injection volume of 1 μL, a split ratio of 10 ∶ 1, a flow rate of 1.0 mL ·min-1, and an inlet temperature of 200 ℃.
    RESULTS A total of 134 non-volatile chemical components and 23 volatile components were analyzed and identified from Yin-Qiao-Qing-Re Tablets, among which 49 compounds were confirmed through comparison with reference standards. The non-volatile components mainly include 27 flavonoids, 21 organic acids, 15 lignans, 14 iridoids, 12 phenylethanoid glycosides, 11 saponins, 10 alkaloids, 5 terpenes, 4 amino acids, 3 phenylpropanoids, 3 nucleosides, 3 xanthones, 3 phenolic glycosides, 2 chromones and 1 carbohydrate. The volatile components mainly include 11 monoterpenes, 5 alcohols and phenols, 3 alkenes, 2 ketones, 1 ester, and 1 hydrocarbon.
    CONCLUSION This study rapidly identifies the chemical components of Yin-Qiao-Qing-Re Tablets, laying a preliminary foundation for research on the pharmacodynamic substances of Yin-Qiao-Qing-Re Tablets and the improvement of quality control standards.

     

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