胶束电动毛细管色谱法同时测定阿咖酚散中3种有效成分  

Simultaneous Separation and Determination of Three Active Ingredients in Paracetamol Caffeine Aspirin Powder by Micellar Electrokinetic Capillary Chromatography

作　　者：陈冰[1,2] 李健[3] 蓝洁 邓庆行 黄碧燕 

机构地区：[1]湛江师范学院化学科学与技术学院,广东湛江524048 [2]广东高校新材料工程技术开发中心,广东湛江524048 [3]湛江师范学院基础教育学院,广东湛江524048

出　　处：《分析测试学报》2012年第6期720-724,共5页Journal of Instrumental Analysis

基　　金：广东省科技计划项目(粤科规划字[2011]97号);湛江市科技招标项目(湛科[2008]74号)

摘　　要：建立了胶束电动毛细管色谱同时分离测定阿咖酚散中咖啡因、对乙酰氨基酚、阿司匹林3种有效成分的方法。对以有机碱三乙醇胺为改进剂的胆酸胶束相进行了优化,对改进剂的影响机理进行了详细讨论。最佳电泳条件如下:以40 mmol/L硼酸盐-60 mmol/L胆酸-12.5%三乙醇胺(pH 12.0)为缓冲体系,分离电压为15 kV,检测波长为254 nm。在上述条件下,14 min内实现了阿咖酚散中3组分的基线分离。咖啡因、对乙酰氨基酚和阿司匹林的线性范围分别为18.75～900.0(r=0.999 9)、2.60～62.50(r=0.992 9)、79.17～3 800 mg/L(r=0.994 0)。上述3组分迁移时间和峰高的相对标准偏差分别不高于1.8%和6.8%。咖啡因、对乙酰氨基酚和阿司匹林的检出限分别为4.6、0.17、38 mg/L。应用该法测定阿咖酚散中上述3组分,加标回收率分别为100%、100%和102%,可满足实际样品分析要求。所建立的方法简便、快速、灵敏、经济,能同时进行阿咖酚散中多种成分的分离测定。A micellar electrokinetic capillary chromatographic （MECC） method was established for the separation and determination of three active components, including caffeine, paracetamolum and aspirin, in Paracetamol Caffeine Aspirin Powder. The micellar phase of cholic acid combined with improver of organic base triethanolamine was optimized. The optimal electrophoretic conditions were as follows： buffer： 40 mmol/L borate - 60 mmol/L cholic acid - 12.5% triethanolamine （ pH 12.0） , separated voltage： 15 kV, detection wavelength： 254 nm. Under the optimum conditions, the baseline separation of three components in Paracetamol Caffeine Aspirin Powder was achieved within 14 min. The linear calibration curves were in the ranges of 18. 75 -900. 0 mg/L （r =0. 999 9） for caffeine, 2.60 - 62.50 mg/L （ r = 0. 992 9 ） for paracetamolum and 79. 17 - 3 800 mg/L （ r = 0. 994 0） for aspirin. The relative standard deviations of three components were no more than 1.8% for migration time and 6.8% for peak height. The detection limits （S/N = 3 ） were 4.6, 0. 17, 38 mg/L, respectively. The spiked recoveries of three components in Paracetamol Caffeine Aspirin Powder were 100% , 100% and 102% , respectively, which could meet the requirement for analyzing reality sample. The improved method is simple, reliable, sensitive and economical, and is suitable for the separation and determination der.

关 键 词：胶束电动毛细管色谱 阿咖酚散 咖啡因 对乙酰氨基酚 阿司匹林 

分 类 号：O657.8[理学—分析化学] TQ460.72[理学—化学]