液质联用法测定消癥散结止痛膏中丝石竹皂苷元-3-O-β-D-葡萄糖醛酸甲酯的含量  

Determination of Gypsogenin-3-O-β-D-glucuronide Methyl Ester in Xiaozheng Sanjie Zhitong Plaster by LC-MS/MS

作　　者：李升 郑枫[1,2,3] LI Sheng;ZHENG Feng(Department of Pharmaceutical Analysis,China Pharmaceutical University,Jiangsu Nanjing 211198;Zhejiang Center for Safety Study of Drug Substances(Industrial Technology Innovation Platform),Zhejiang Hangzhou 310018;Key Laboratory of Drug Quality Control and Pharmacovigilance,Ministry of Education,Jiangsu Nanjing 210009,China)

机构地区：[1]中国药科大学药物分析系,江苏南京211198 [2]浙江省原料药安全研究中心(工艺技术创新平台),浙江杭州310018 [3]药物质量与安全预警教育部重点实验室,江苏南京210009

出　　处：《广州化工》2024年第24期103-106,共4页GuangZhou Chemical Industry

摘　　要：建立液质联用检测法测定消癥散结止痛膏中丝石竹皂苷元-3-O-β-D-葡萄糖醛酸甲酯的含量。采用反相C_(18)色谱柱,以乙腈-1%甲酸水溶液为流动相进行梯度洗脱;质谱采用电喷雾离子源(ESI),正离子、多重反应监测模式检测。丝石竹皂苷元-3-O-β-D-葡萄糖醛酸甲酯在0.10~2.06μg·mL^(-1)浓度范围内线性关系良好,R^(2)=0.9997;平均回收率在89.6%~91.7%之间,RSD为9.30%;定量限为102.9 ng·mL^(-1)。本方法专属性好、灵敏度高,适用于消癥散结止痛膏中丝石竹皂苷元-3-O-β-D-葡萄糖醛酸甲酯的测定。To determine gypsogenin-3-O-β-D-glucuronide methyl ester in Xiaozheng Sanjie Zhitong plaster by LC-MS/MS.RP-C_(18) column was used,with the mobile phase of acetonitrile and 1%formic acid solutionby gradient elution.The mass spectrometer was equipped with an electrospray ion source and was operated in positive ion mode with multiple reaction monitoring.The linear range of gypsogenin-3-O-β-D-glucuronide methyl ester was 0.10 to 2.06μg·mL^(-1)(R^(2)=0.9997).The average recovery was range of 89.6%to 91.7%,with RSD was 9.30%.The LOQ was 102.9 ng·mL^(-1).The method is specific and sensitive for the determination of gypsogenin-3-O-β-D-glucuronide methyl ester in Xiaozheng Sanjie Zhitong plaster.

关 键 词：液质联用 消癥散结止痛膏 丝石竹皂苷元-3-O-β-D-葡萄糖醛酸甲酯 

分 类 号：R917[医药卫生—药物分析学]