UPLC-MS/MS法同时定量分析暖宫孕子胶囊中的10个成分

Simultaneous determination of ten components in Nuangong Yunzi capsules by UPLC-MS/MS

目的:建立UPLC-MS/MS法同时测定暖宫孕子胶囊中没食子酸、松脂醇二葡萄糖苷、芍药内酯苷、毛蕊花糖苷、芍药苷、黄芩苷、川续断皂苷Ⅵ、苯甲酰芍药苷、藁本内酯、α-香附酮10个成分的含量。方法:采用Acquity UPLC BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm),流动相为乙腈-0.1%甲酸水溶液,梯度洗脱;定量分析采用多反应离子检测模式(MRM)。结果:各化合物在相应质量浓度范围内呈良好的线性关系,r值为0.995 3~0.999 8;10个成分的精密度RSD在0.5%~6.2%间,平均加样回收率为92.4%~103.4%,相应的RSD在1.8%~6.5%间。6批样品中没食子酸、松脂醇二葡萄糖苷、芍药内酯苷、毛蕊花糖苷、芍药苷、黄芩苷、川续断皂苷Ⅵ、苯甲酰芍药苷、藁本内酯、α-香附酮10个成分的含量范围分别为101.4~135.8、18.3~28.7、711.1~769.7、163.9~236.6、1 573.2~1 622.4、592.4~749.8、506.8~537.9、25.6~34.6、3 400.8~4 594.3、55.5~63.2μg·g^(-1)。结论:所建立的方法可用于暖宫孕子胶囊制剂的质量控制及生产过程控制。

Objective：To establish a UPLC-MS/MS method for the simultaneous determination of gallic acid,pinoresinol diglucoside,albiflorin,verbascoside,paeoniflorin,baicalin,asperosaponinⅥ,benzoylpaeoniflorin,ligustilide andα-cyperone in Nuangong Yunzi capsules.Methods：An acquity UPLC BEH C_（18）（2.1 mm×50 mm,1.7μm）column was used.The gradient mobile phase consisted of acetonitrile and 0.1%formic acid.Mass data acquisition was performed with multiple reaction monitoring（MRM）.Results：Excellent linear calibration curves were obtained over the tested concentration ranges（r=0.995 3-0.999 8）.Intra-and inter-day precisions（RSD）were between 0.5%and 6.2%.The mean recoveries were all between 92.4%and 103.4%,and the RSD values were1.8%-6.5%.The contents of gallic acid,pinoresinol diglucoside,albiflorin,verbascoside,paeoniflorin,baicalin,asperosaponinⅥ,benzoylpaeoniflorin,ligustilide andα-cyperone in 6 samples were 101.4-135.8μg·g^（–1）,18.3-28.7μg·g^（–1）,711.1-769.7μg·g^（–1）,163.9-236.6μg·g^（–1）,1 573.2-1 622.4μg·g^（–1）,592.4-749.8μg·g^（–1）,506.8-537.9μg·g^（–1）,25.6-34.6μg·g^（–1）,3 400.8-4 594.3μg·g^（–1） and 55.5-63.2μg·g^（–1）,respectively.Conclusion：This method can be used for quality control and process control of Nuangong Yunzi capsules.