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目的:建立HPLC-ESI-Q-TOF-MS同时鉴定消癌解毒方水提液中化学成分的方法,并使用UPLC-TQMS技术同时测定其中芦丁和半枝莲碱B含量。方法:ZORBAX SB-C18色谱柱(4.6mm×150mm,5μm)用于成分定性分析,流动相为乙腈(A)-0.1%甲酸溶液(B)梯度洗脱,正离子模式下采集数据。定量分析使用Waters ACQUITY UPLC BEH-C18色谱柱(2.1mm×100mm,1.7μm),0.1%甲酸水溶液(A)-乙腈(B)梯度洗脱,正、负离子检测模式。结果:消癌解毒方水提液中鉴定出20种化学成分,并同时测定其中芦丁和半枝莲碱B等成分含量,2种成分在测定的线性范围内线性关系良好,R2>0.9995,加样回收率98.88%、98.01%(RSD<3%)。结论:该方法能够快速、简便、高效地对消癌解毒方中化学成分进行定性、定量分析。
OBJECTIVE: To establish a HPLC-ESI-Q-TOF-MS method for the simultaneous determination of chemical constituents in Xiaojian Jiedu Fang aqueous extract, and to determine the content of rutin and Scutellaria B together by UPLC-TQMS. Methods: ZORBAX SB-C18 column (4.6mm × 150mm, 5μm) was used for the qualitative analysis of components. The mobile phase consisted of acetonitrile (A) -0.1% formic acid solution (B) gradient elution. Quantitative analysis was performed on a Waters ACQUITY UPLC BEH-C18 column (2.1 mm × 100 mm, 1.7 μm) with a gradient of 0.1% formic acid in water (A) -acetonitrile (B), positive and negative ion detection mode. Results: 20 kinds of chemical constituents were identified from the aqueous extract of Xiaoyan Jiedu Fang, and the content of rutin, Scutellaria B and so on were determined at the same time. The linearity of the two components in the determination range was good, R2> 0.9995, The recoveries of samples were 98.88% and 98.01% (RSD <3%). Conclusion: This method can be used to qualitatively and quantitatively analyze the chemical constituents in Xiaojianjiedu Fang quickly, easily and efficiently.