摘要
建立了以离子液体为添加剂的反向微乳毛细管电泳(IL—MEEKC)法分离测定化妆品中氢化可的松、泼尼松和醋酸氢化可的松3种糖皮质激素的方法。微乳毛细管电泳的最佳缓冲体系组成为:2.4%SDS+6.6%正丁醇+0.5%正辛烷+35mmol/L BMIM—BF4+20mmol/L磷酸二氢钠缓冲液(pH2.2);运行电压-20kV,检测波长250nm。在优化实验条件下,氢化可的松、泼尼松和醋酸氢化可的松分别在5~400、5~400、5—800mg·L^-1范围内线性良好,检出限(S/N=3)分别为0.9、0.9、1.2mg/L,相对标准偏差不大于4.3%,平均加标回收率分别为102%、97%和94%。结果表明,利用离子液体作为添加剂的反向微乳毛细管电泳方法分离3种糖皮质激素比常规的MEEKC具有更高的分离度。该方法快速、灵敏、有效,已成功用于实际样品中糖皮质激素的检测。
A reversed microemulsion electrokinetic chromatographic (MEEKC) method was developed for the separation of three corticosteroids, including hydrocortisone, prednisone and hydrocortisone acetate by using 1 -butyl-3-methylimizolium tetrafluoborate ( BMIM - BF4 ) ionic liquid (IL) as additive. The effects of experimental conditions such as BMIM - BF4 concentration and pH value on separation efficiency were investigated. The optimized conditions were as follows: 2.4% sodium dodecyl sulfate(SDS) , 6.6% 1-butanol, 0. 5% n-octane, 35 mmol/L BMIM - BF4, pH 2.2 20 mmol/L NaH2PO4, an applied voltage of - 20 kV and a detection wavelength of 250 nm. Under the optimized conditions, the calibration curves were linear in the range of 5 - 400, 5 - 400, 5 - 800 mg · L^-1 for hydrocortisone, prednisone and hydrocortisone acetate with detection limits ( S/N = 3 ) of 0. 9, 0. 9, 1.2 mg/L, respectively. The RSDs(n =3) were less than 4.3%. The average spiked recoveries were 102% , 97% and 94% , respectively. The results showed that the resolution of the IL - MEEKC method for the separation of hydrocortisone, prednisone and hydrocortisone acetate was higher than that of the conventional MEEKC method. The proposed method was simple, rapid and effective, and could be used for the quality control of cosmetics.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第2期203-206,212,共5页
Journal of Instrumental Analysis
基金
国家自然科学基金资助项目(20775028)
江南大学青年基金资助项目(20070337)
关键词
微乳毛细管电泳
糖皮质激素
离子液体
化妆品
microemulsion electrokinetic chromatography
corticosteroids
ionic liquid
cosmetics