超高效液相色谱法同时测定化妆品中多种雌激素

建立了化妆品中5种雌激素(己烯雌酚、17-α-雌二醇、17-β-雌二醇、己烷雌酚、17-α-乙炔雌二醇)的超高效液相色谱(UPLC)测定方法。化妆品样品采用氯化钠饱和溶液分散,然后用乙腈从分散液中提取雌激素类药物,用亚铁氰化钾和醋酸锌从提取液中沉淀大分子,OasisHLB固相萃取小柱富集净化,以W aters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm)分离,经乙腈-水为流动相梯度洗脱,5 m in内完成5种雌激素的分离及检测。在0.5~8.0 mg/L进样质量浓度范围内,5种雌激素的工作曲线的线性相关系数均高于0.999 5;在0.10,0.20,0.50 mg/kg 3个添加水平下5种雌激素的平均回收率为83.1%~95.4%,相对标准偏差小于7.4%。

Determination of estrogens in cosmetics by ultrahigh performance liquid chromatography

A method was established for the determination of five estrogens(diethylstilbestrol,17-α-estradiol,17-β-estradiol,dihydroethylstilbestrol and 17-α-ethinyl estradiol) in cosmetics by ultrahigh performance liquid chromatography(UPLC).The cosmetic sample was firstly dispersed by saturated NaCl solution and then the dispersion was extracted with acetonitrile.The extract was treated by potassium ferrocyanide and zinc acetate to cause the precipitation of big molecular compounds.The clear phase was enriched and purified by a Oasis HLB solid phase extraction cartridge.Then the five estrogens were separated and detected within 5 min on a chromatograph column of Waters ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7 μm) by gradient elution with acetonitrile-water system.In the range of 0.5~8.0 mg/L,the calibration curves of five estrogens show good linearity with the correlation coefficients larger than 0.999 5.The mean recoveries at the three spike levels(0.10,0.20,0.50 mg/kg) were 83.1%~95.4% with less than 7.4% of relative standard deviations.