UPLC-MS/MS法测定咳速停糖浆中3种兴奋剂类生物碱  

Simultaneous determination of three stimulant alkaloids in Kesuting Syrupy by UPLC-MS /MS

作　　者：朱平川[1] 岑卫健[1] 范晓苏[2] 

机构地区：[1]广西大学亚热带农业生物资源保护与利用国家重点实验室,广西南宁530004 [2]广西大学化学化工学院,广西南宁530004

出　　处：《中成药》2014年第5期970-973,共4页Chinese Traditional Patent Medicine

基　　金：广西自然科学基金项目(桂科自0832034);广西大学科研基金项目(DD703003)

摘　　要：目的建立同时测定咳速停糖浆中盐酸麻黄碱、盐酸伪麻黄碱以及磷酸可待因3种有效成分的量的超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法。方法用Agilent Zorbax RRHD Eclipse Plus C18（50 mm×2.1 mm,1.8μm）色谱柱,以甲醇-0.1%甲酸的水溶液为流动相,体积流量0.30 mL/min。在电喷雾电离（ESI）正离子模式下,采用的是多重反应监测模式（MRM）进行检测。结果盐酸麻黄碱、盐酸伪麻黄碱以及磷酸可待因的线性范围分别为0.001 6～4.5 mg/L、0.000 8～4.8 mg/L、0.004～2.0 mg/L;检出限分别为0.8μg/L、0.4μg/L、1.2μg/L;3种成分的加样回收率为91.1%～104%;相对标准偏差均不大于2.6%。结论该方法简便、准确、快速、灵敏度高,已成功地用于实际的样品分析。AIM A method for simultaneous determination of ephedrine hydrochloride,pseudoephedrine hydrochloride and codeine phosphate in Kesuting Syrupy was established by ultra performance liquid chromatography with tandem mass spectrometry（ UPLC-MS / MS）. METHODS The UPLC separation was performed on a Zorbax RRHD Eclipse Plus C18column（ 2. 1 mm × 50 mm,1. 8 μm） by using methanol and water which contained 0. 1% formic acid as mobile phase with the gradient elution at a flow rate of 0. 30 mL / min. The analytes were detected by tandem mass spectrometry under the positive ion mode with the ESI source and carried out in the multiple reaction monitoring（ MRM） mode. RESULTS Under the optimum conditions,the calibration curves were linear in the range of 0. 001 6- 4. 5 mg / L for ephedrine hydrochloride,0. 000 8- 4. 8 mg / L for pseudoephedrine hydrochloride,0. 004- 2. 0 mg / L for codeine phosphate. The detection limits were 0. 8,0. 4,1. 2 μg / L,respectively. The average recoveries of the three effective components were between 91. 1% and 104% with all relative standard deviations not more than 2. 6%. CONCLUSION The developed method is simple,rapid and accurate,and suitable for the quality control of the three components in Kesuting Syrupy.

关 键 词：咳速停糖浆 生物碱 超高效液相色谱-串联质谱(UPLC-MS MS) 

分 类 号：R927.2[医药卫生—药学]