微乳毛细管电色谱电动进样-场放大堆积法检测化妆品中糖皮质激素  

Determination of Glucocorticoids in Cosmetics by Microemulsion Electrokinetic Chromatography With Electric Injection and Field-amplified Sample Stacking

作　　者：孙雪婷[1] 商少明[1] 陈秀英[1] 汪云[1] 李娟[1] 

机构地区：[1]江南大学化学与材料工程学院食品胶体与生物技术教育部重点实验室,无锡214122

出　　处：《分析化学》2014年第1期36-40,共5页Chinese Journal of Analytical Chemistry

基　　金：国家质量检验检疫监督总局项目(No.2010IK183)资助

摘　　要：采用反向微乳毛细管电色谱电动进样联用场放大堆积，建立了在线富集检测化妆品中6种糖皮质激素分析方法。微乳毛细管电色谱缓冲体系为2．4％（w／w）十二烷基硫酸钠，6．6％（w／w）正丁醇，0．6％（w／w）正辛烷，20mmol／L磷酸盐缓冲液（pH2．2），分离电压-20kV，进样-20kVx54s，进水15kPax40S，检测波长240nm。讨论了样品基质、进样时间和电压、水柱长度对富集效果的影响。在优化条件下，6种激素的富集倍数分别为100～186倍，在0．05～15．0mg／L范围内呈线性关系，相关系数0．9986～0．9997。检出限为20—60μg/L（S／N=3），标准加入量为50μg／L时平均回收率85．9％-103．8％，相对标准偏差均小于5．8％。迁移时间和峰高的日内精密度分别为2．2％和7．9％，13间精密度分别为2．9％和9．0％。Reverse migration microemulsion electrokinetic chromatography combined with electric injection and field-amplified sample stacking has been developed for the determination of 6 glucocorticoids in cosmetics. The microemulsion background buffer was composed of 2.4% （w/w） dodecyl sodium sulfate, 6. 6% （w/w） butanol, 0.6% （w/w） octane, 20 mmoL/L NaH2PO4 buffer （pH 2.2）. Separating voltage was -20 kV. The conditions of sample injection and water plug were -20 kV × 54 s and 15 kPa×40 s, respectively. Detection wavelength was at 240 nm. Several parameters were discussed including sample matrix, the length of sample injection and water plug. Under the optimum conditions, the enrichment factors of 100-186 were achieved. The calibration curves were linear at the concentration of 0. 05 to 15.0 mg/L with correlation coefficients of 0. 9986-0. 9997. The limit of detections were 20-60 μg/L （S/N = 3 ）. Mean recoveries at the spiked level of 50 μg/L ranged from 85.9% to 103.8%, with the relative standard deviation less than 5.8%. The RSDs of migration time and peak height were 2.2% and 7.9% （intraday）, 2.9% and 9.0% （interday）, respectively.

关 键 词：反向微乳毛细管电色谱 电动进样 场放大堆积 富集 糖皮质激素 化妆品 

分 类 号：O657.1[理学—分析化学] TQ658[理学—化学]