UPLC-MS/MS法同时测定黄芩中8种主要指标性成分的含量

Simultaneously Determination of Eight Components in Schisandra chinensis Georgi by UPLC-MS/MS

目的采用超高效液相-三重四级杆串联质谱（UPLC-MS/MS）的方法,对黄芩中的黄芩素、黄芩苷、汉黄芩素、汉黄芩苷、木蝴蝶素A、木蝴蝶苷A、白杨素、芹菜素进行定量检测。方法采用Thermo BDS Hypersil C18（2.1mm×100mm,2.3μm）色谱柱进行色谱分离,柱温为40℃,流动相为乙腈（A）和0.1%甲酸水（B）,梯度洗脱,流速为0.25mL/min,采用多反应监测的方法进行质谱扫描。结果白杨素、黄芩素、芹菜素、木蝴蝶素A、汉黄芩素、黄芩苷、汉黄芩苷、木蝴蝶苷A的定量范围分别为0.975-62.5ng/mL（r2=0.999 8）、4.875-2 500ng/mL（r2=0.999 7）、0.975-62.5ng/mL（r2=0.999 4）、0.097 5-12.5ng/mL（r2=0.999 6）、0.048 83-6.25ng/mL（r2=0.999 9）、4.875-2 500ng/mL（r2=0.999 8）、0.488 3-250ng/mL（r2=0.999 9）、0.488 3-250ng/mL（r2=0.999 8）,在该范围内线性关系良好;8种指标性黄酮成分的回收率（n=6）分别为98.75%、96.44%、101.13%、99.41%、102.26%、98.45%、96.75%、99.42%;检测方法的重现性和稳定性良好。结论所建立的分析方法操作简便、快速、灵敏,结果准确,重复性好,所需样品少,可应用于黄芩中这8种成分的检测。

OBJECTIVE To develop a sensitive and selective ultra performance liquid chromatography-triple quadrupole mass spectrometer（UPLC-MS/MS）method for quantification of eight components（chrysin,baicalein,apigenin,orohylin A,wogonin,baicalin,wogonoside,oroxin A）in Schisandra chinensis Georgi.METHODS The separation was performed on a Thermo BDS Hypersil C18（2.1mm×100mm,2.3μm）column.The mobile consisted of acetonitrile（A）and 0.1% formic acid aqueous with a gradient elution at a flow-rate of 0.25mL/min.The detection was acquired by MRM.The column temperature was 40℃.RESULTS The linear ranges of chrysin,baicalein,apigenin,orohylin A,wogonin,baicalin,wogonoside,oroxin A were 0.975-62.5ng/mL（r2=0.999 8）,4.875-2 500ng/mL（r2=0.999 7）,0.975-62.5ng/mL（r2=0.999 4）,0.097 5-12.5ng/mL（r2=0.999 6）,0.048 83-6.25ng/mL（r2=0.999 9）,4.875-2 500ng/mL（r2=0.999 8）,0.488 3-250ng/mL（r2=0.999 9）,0.488 3-250ng/mL（r2=0.999 8）,respectively.The recoveries were 98.75%,96.44%,101.13%,99.41%,102.26%,98.45%,96.75%,99.42%.CONCLUSION The proposed method enables quantification for the study of the compounds of chrysin,baicalein,apigenin,orohylin A,wogonin,baicalin,wogonoside,oroxin A in Schisandra chinensis Georgi