HPLC-MS法同时测定防芷鼻咽颗粒中6个成分的含量  

Simultaneous determination of 6 compounds in Fangzhi nasopharyngeal granules by HPLC-MS

作　　者：刘灵改[1] 支旭然[2] 郭进[1] 王捧英[3] 胡玉录[1] 任非[1] 张兰桐[2] 孟岩[2] 

机构地区：[1]河北医科大学第二医院药剂科,石家庄050000 [2]河北医科大学药学院药物分析教研室,石家庄050017 [3]河北医科大学西山校区,石家庄050228

出　　处：《药物分析杂志》2014年第5期830-835,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：河北省科技支撑计划项目(132777105D)

摘　　要：目的：采用HPLC-MS法同时测定防芷鼻咽颗粒中升麻素苷、丹皮酚、木兰脂素、欧前胡素、异欧前胡素和黄芪甲苷的含量。方法：采用Dikma Diamonsil C18色谱柱（150 mm×4.6 mm,5μm）,柱温为室温,以甲醇-0.05%甲酸水溶液（v/v）为流动相进行梯度洗脱（0～6 min,25%A→75%A;6～10 min,75%A→95%A;10～15 min,95%A）,流速0.8 mL·min-1,进样量20μL;采用电喷雾离子源进行正离子模式监测,多反应监测模式（MRM）用于定量分析。结果：在15 min内,防芷鼻咽颗粒中6个成分（升麻素苷、丹皮酚、木兰脂素、欧前胡素、异欧前胡素和黄芪甲苷）完全分离;峰面积与浓度有良好的线性关系;平均加样回收率为98.9%～100.7%,精密度RSD为0.88%～1.2%。结论：该方法经方法学验证可用于防芷鼻咽颗粒中多种成分的含量测定和质量控制。Objective： To develop a method for the simultaneous determination of prim-O-glucosylcimifugin,paeonol,magnolin,imperatorin,isoimperatorin and astragaloside Ⅳ in Fangzhi nasopharyngeal granules by HPLC-MS / MS. Methods： The samples were separated on a Diamonsil C18column（ 150 mm × 4. 6 mm,5 μm）,by a gradient elution（ 0-6 min,25% A→75% A; 6-10 min,75% A→95% A; 10-15 min,95% A） using methanol and 0. 05%（ v/v） aqueous formic acid as the mobile phase at a flow rate of 0. 8 mL·min-1; the injection volume was 20 μL. The column temperature was room temperature. Multiple-reaction monitoring（ MRM） scanning was employed for quantification with switching electrospray ion source polarity in positive mode. Results： The complete separation was obtained within 15 min for the 6 compounds（ prim-O-glucosylcimifugin,paeonol,magnolin,imperatorin,isoimperatorin and astragaloside Ⅳ）. The regression equations showed good linear relationship between the peak area and the content of each compound. The average recoveries ranged from 98. 9% to 100. 7%,and the precision in terms of RSD was in the range of 0. 88%-1. 2%. Conclusion： The methodology validation shows that the method can be used for the determination of 6 compounds in Fangzhi nasopharyngeal granules.

关 键 词：液质联用(HPLC-MS) 防芷鼻咽颗粒 升麻素苷 丹皮酚 木兰脂素 欧前胡素 异欧前胡素 黄芪甲苷 

分 类 号：R286.0[医药卫生—中药学]