基于LC-MS/MS法的玄麦甘桔颗粒中麦冬及山麦冬的检查

Inspection of Ophiopogonis Radix and Liriopes Radix in Xuanmai Ganjie Granules by LC-MS/MS

目的:建立玄麦甘桔颗粒中麦冬有效成分甲基麦冬黄烷酮A和甲基麦冬黄烷酮B及山麦冬特征性成分山麦冬皂苷B和短葶山麦冬皂苷C的检查方法,并对市售不同厂家、不同批号的玄麦甘桔颗粒进行检测和分析。方法:采用液相色谱-串联三重四级杆质谱仪(LC-MS/MS),ACQUITY UPLC BEH C18柱(2.1 mm×100 mm,1.7 μm),流动相为乙腈和0.1%甲酸溶液,流速0.3 mL/min,采用正负离子同时监测,多反应监测模式扫描。结果:上述4种成分分别在24.07~1203.52、10.58~529.13、8.31~415.70、9.11~455.71 ng/mL内线性关系良好(r>0.999 0),加样回收率为91.1%~103.2%,RSD均小于3.0%;30批玄麦甘桔颗粒中,3批检出山麦冬皂苷B和短葶山麦冬皂苷C。结论:此方法选择性强、灵敏度及准确度高,操作简便,可快速、有效地评价玄麦甘桔颗粒中麦冬的质量。

Objective:To establish a method for determining methylophiopogonanone A,methylophiopogonanone B of ophiopogonis radix and liriopesides B,liriope muscari baily saponins C of liriopes radix in xuanmai ganjie granules,detection and analysis of different manufacturers,different batches of xuanmai ganjie granules.Methods:Xuanmai ganjie granules were determined by LC-MS/MS in MRM mode with simultaneous monitoring by positive and negative ions.The chromatographic separation was achieved on ACQUITY UPLC BEH C18 column (2.1 mm×100 mm,1.7 μm),the mobile phase was acetonitrile and 0.1% formic acid aqueous solution,the flow rate was 0.3 mL/min and the injection volume was 5 μL.Results:The above four ingredients showed good linearity (r>0.999 0) in the ranges of 24.07-1 203.52,10.58-529.13,8.31-415.70,9.11-455.71 ng/mL.The average recoveries were between 93.1%-103.2% (RSD<3.0%).In the 30 batches of xuanmai ganjie granules,liriopesides B and liriope muscari baily saponins C were detected in 3 batches.Conclusion:The developed method is sensitive,accurate and easy to operate,and can be used for the quality evaluation of ophiopogonis radix in xuanmai ganjie granules rapidly and effectively.