LC-MS/MS测定养血清脑颗粒中9个蒽醌成分的含量

Determination of nine anthraquinone constituents in Yangxue Qingnao Granules via LC-MS/MS

目的采用LC-MS/MS方法对养血清脑颗粒中大黄酸、大黄素、大黄素甲醚、芦荟大黄素、橙黄决明素、甲基钝叶决明素、钝叶素、大黄素-8-O-葡萄糖苷、大黄素甲醚-8-O-葡萄糖苷,共9个蒽醌成分进行定量分析。方法色谱柱为Agilent Zorbax SB-C_(18)(4.6mm×100mm,1.8μm),流动相为水(含0.1%甲酸)-乙腈,线性梯度洗脱,流速0.4ml/min,采用ESI负离子电离方式,MRM扫描模式进行检测。结果养血清脑颗粒中9个蒽醌成分具有较好的线性关系(R^2>0.98),各成分回收率为95.6%~105.5%,批内、批间精密度和准确度良好,9个蒽醌成分的含量之和为366μg·g^(-1)。结论该方法操作简便、灵敏度高、分析速度快,可用于养血清脑颗粒中多个蒽醌成分的同时测定。

Objective A quantitative LC-MS/MS method was developed for nine anthraquinone constituents including rhein,emodin,physcion,aloe-emodin,aurantio-obtusin,chryso-obtusin,obtusifolin,emodin-8-O-glucoside,physcion-8-O-glucoside in Yangxue Qingnao granules. Methods The sample was separated on Agilent Zorbax SB-C_（18）column（ 4. 6mm ×100mm,1. 8μm） and the flow rate was 0. 4m L/min with water（ containing 0. 1% formic acid）-acetonitrile as the mobile phase in gradient elution mode. The detection was performed on a triple quadrupole tandem mass spectrometer with electrospray ionization（ ESI） source using multiple reaction monitoring（ MRM） mode in negative mode. Results Nine anthraquinones in Yangxue Qingnao granules showed good linearity（ R^2 0. 98）. The average recoveries of each component were from 95. 6% to105. 5%. Good precision and accuracy（ intra-assay and inter-assay） were obtained. The content of nine anthraquinones was366 μg·g-1. Conclusion The simple,sensitive,rapid approach enables simultaneous determination the contents of anthraquinones in Yangxeu Qingnao granules.