固相萃取-微乳液相色谱法对化妆品中8种激素的同时测定

Simultaneous Determination of 8 Hormones in Cosmetics by Solid Phase Extraction with Microemulsion Liquid Chromatography

建立了固相萃取-微乳液相色谱同时测定化妆品中糖皮质激素、雌激素、雄激素、孕激素等8种激素药物的新方法。化妆品样品用甲醇超声提取，经Cleanert ODS—SPE固相萃取柱纯化后，以Venusil ASB C8（T）（4．6mm×200mm，5μm，30nm）为色谱柱，3．0％十二烷基硫酸钠（SDS）-6．6％正丁醇-0．8％正辛烷-89．6％水为流动相，检测波长为240nm。结果表明，8种激素在15min内达到基线分离，线性范围为0．5—30mg／L，相关系数r均大于0．9995。在低、中、高3种加标水平下，8种激素的平均回收率为82％～109％；相对标准偏差为1．5％～5．4％：检出限为0．04～0．07ng。

A new analytical method based on solid phase extraction couple with microemulsion liquid chromatography has been developed for the simultaneous determination of 8 hormones in cosmetics samples. The samples were extracted with methanol under ultrasonication, and then cleaned up by a Cleanert ODS solid phase extraction cartridge. 8 hormones were separated within 15 min on a Venusil ASB Cs（T） （4. 6 mm ×200 mm, 5 μm, 30 nm） column by the mobile phase consisted of microemulsion 3.0% sodium dodecylsulfate （SDS） - 6.6% n-butanol - 0. 8% n-octane - 89.6% water, and detected at 240 nm. The calibration curves of 8 hormones were linear in the range of 0. 5 - 30 mg/L with correlation coefficients more than 0. 999 5. The average spiked recoveries for 8 hormones ranged from 82% to 109% with relative standard deviations of 1.5% - 5.4% , and the limits of detection were in the range of 0. 04 - 0. 07 ng.