高效液相色谱-串联质谱法测定葛根芩连片中染色剂金胺O的方法研究

中国药物警戒 ›› 2016, Vol. 13 ›› Issue (4): 216-218.

高效液相色谱-串联质谱法测定葛根芩连片中染色剂金胺O的方法研究

朱雪妍,谷立勍,何颂华

广西食品药品检验所,广西南宁 530021

收稿日期:2015-12-03 修回日期:2016-06-30 出版日期:2016-04-20 发布日期:2016-06-30
作者简介:朱雪妍，女，硕士，主管药师,中药民族药的质量标准分析与研究。

Study on Determination of Dye Auramine O in Gegen Qinlian Tablets by HPLC-MS/MS

ZHU Xue-yan, GU Li-qing, HE Song-hua

Guangxi Institute for Food and Drug Control,Guangxi Nanning 530021,China

Received:2015-12-03 Revised:2016-06-30 Online:2016-04-20 Published:2016-06-30

摘要/Abstract

摘要： 目的建立液相色谱-串联质谱法（LC-MS/MS）测定葛根芩连片中染料金胺O的含量。方法采用Agilent Eclipse plus C18 (2.1×100 mm, 1.8μm),流动相:乙腈-0.01 mol·L^-1乙酸铵,梯度洗脱;流速:0.3 mL·min^-1;柱温35 ℃;进样量:2μL。离子源:电喷雾电离源（ESI）;扫描模式:多反应监测（MRM）。结果方法学验证结果表明,金胺O在0.093 4~1.869 pg范围内线性关系良好（r=0.999 9）,平均回收率为94.38%,RSD为3.60%（n=9）。结论本方法准确、便捷,具有良好的精密度、重现性和稳定性,线性关系良好,可用于检测葛根芩连片中染色剂金胺O的含量。

关键词: 葛根芩连片, 液相色谱-串联质谱, 染色剂, 金胺O

Abstract: Objective To establish method for determination of dye auramine O in Gegen Qinlian tablets by LC-MS/MS. Methods Agilent Eclipse plus C18(2.1×100 mm, 1.8μm) was used. A gradient elution program of acetonitrile-0.01 mol·L^-1 ammonium acetate was adopted at the flow rate of 0.3 mL· min^-1. The column temperature was maintained at 35℃ and the sample size was 2 μL. The analyses were detected by an electrospray ionization tandem mass spectrometry with dynamic MRM. Results The results of verification of methodology showed the calibration curve of auramine O was good linear in the range of 0.093 4~1.869 pg (r =0.999 9), and the recovery was 94.38% (RSD=3.60%, n=9). Conclusion The method was convenient, accurate with good precision, reproducibility and stability which has good linear relationship. It can be used for the determination the content of dye auramine O in Gegen Qinlian tablets.

Key words: Gegen Qinlian tablets, LC-MS/MS, dye, auramine O

中图分类号:

R917

朱雪妍,谷立勍,何颂华. 高效液相色谱-串联质谱法测定葛根芩连片中染色剂金胺O的方法研究[J]. 中国药物警戒, 2016, 13(4): 216-218.

ZHU Xue-yan, GU Li-qing, HE Song-hua. Study on Determination of Dye Auramine O in Gegen Qinlian Tablets by HPLC-MS/MS[J]. Chinese Journal of Pharmacovigilance, 2016, 13(4): 216-218.

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