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

  • 摘要: 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(2.1mm×100mm,2.3μm)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0.25mL/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0.975~62.5ng/mL(r=0.9998)、4.875~2500ng/mL(r=0.9997)、0.975~62.5ng/mL(r=0.9994)、0.0975~12.5ng/mL(r=0.9996)、0.04883~6.25ng/mL(r=0.9999)、4.875~2500ng/mL(r=0.9998)、0.4883~250ng/mL(r=0.9999)、0.4883~250ng/mL(r=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。

     

    Abstract: 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 (2.1mm×100mm, 2.3μm) column. The mobile consisted of acetonitrile (A) and 0.1% formic acid aqueous with a gradient elution at a flow-rate of 0.25mL/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 0.975~62.5ng/mL (r=0.9998), 4.875~2500ng/mL (r=0.9997), 0.975~62.5ng/mL (r=0.9994), 0.0975~12.5ng/mL (r=0.9996), 0.04883~6.25ng/mL (r=0.9999), 4.875~2500ng/mL (r=0.9998), 0.4883~250ng/mL (r=0.9999), 0.4883~250ng/mL(r=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

     

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