光叶丁公藤中化学成分的UPLC-Q-Exactive Focus-MS/MS鉴定

Identification of Chemical Constituents in Caulis of Erycibe schmidtii by UPLC-Q-Exactive Focus-MS/MS

目的:利用UPLC-Q-Exactive Focus-MS/MS技术对光叶丁公藤中的化学成分进行快速识别和鉴定。方法:选用80%甲醇提取光叶丁公藤作为供试品溶液,对光叶丁公藤药材的化学成分进行分析和鉴定。采用Thermo Accucore aQ C18色谱柱(2.1 mm×150 mm,2.6μm)进行色谱分离,以甲醇(A)-0.1%甲酸水溶液(B)为流动相进行梯度洗脱(0~12 min,5%~25%A;12~20 min,25%~30%A;20~28 min,30%~38%A;28~40 min,38%~42%A);质谱分析采用正、负离子监测模式和加热电喷雾离子源(HESI),扫描范围m/z 80~1200。结果:共鉴定出了42个化学成分,包括香豆素类12个、绿原酸类14个、生物碱类1个、酰胺类1个,其余14个为酯化糖苷类。结论:UPLC-Q-Exactive Focus-MS/MS技术可以快速、全面地鉴定光叶丁公藤药材中的化学成分,其中11个成分经与对照品比对后准确鉴定,31个成分在该植物中属首次发现,2个成分在丁公藤属植物中属首次发现,可为光叶丁公藤的物质基础研究和替代品开发提供重要依据。

Objective:To rapidly recognize and identify the chemical constituents in caulis of Erycibe schmidtii by ultra-high performance liquid chromatography coupled with Q-Exactive Focus mass spectrometry(UPLC-Q-Exactive Focus-MS/MS).Method:Taking 80%methanol extract of E.schmidtii caulis as the test solution,the chemical constituents in caulis of E.schmidtii were analyzed and identified.Thermo Accucure aQ C18 column(2.1 mm×150 mm,2.6μm)was used for chromatographic separation with the mobile phase of methanol(A)-0.1%formic acid solution(B)for gradient elution(0-12 min,5%-25%A;12-20 min,25%-30%A;20-28 min,30%-38%A;28-40 min,38%-42%A).Positive and negative ion monitoring modes and heated electrospray ion source(HESI)were used for mass spectrographic analysis.The scanning range was m/z80-1200.Result:A total of 42 chemical constituents from caulis of E.schmidtii were identified,including 12 coumarins,14 chlorogenic acids,1 tropane alkaloid,1 amide and 14 esterified glycosides.Conclusion:Chemical constituents in caulis of E.schmidtii can be quickly and fully identified by UPLC-Q-Exactive FocusMS/MS.Among them,11 compounds are unambiguously identified by comparing with reference standards,31 compounds are reported for the first time in this herb,2 compounds are reported for the first time in Erycibe plants.This paper can provide the important basis for study on pharmacodynamic material base and substitute development of E.schmidtii caulis.