响应面优化固相微萃取-超高效液相色谱法测定化妆品中7种激素

Optimization of solid phase micro extraction-ultra high performance liquid chromatography for the determination of 7 hormones in cosmetics by response surface optimization methodology

目的采用单因素变化与响应面优化结合的方式对固相微萃取的条件进行优化,建立固相微萃取-超高效液相色谱法测定化妆品中丙酸氯倍他索、己烯雌酚、β-雌二醇、炔雌醇、黄体酮、甲炔诺酮和丙酸睾丸素7种激素的方法。方法样品经乙腈溶液超声提取后,样品提取液在60℃、600 r/min下用85μm PA萃取头直接萃取50 min,乙腈中静态脱附5 min,脱附液经C18液相色谱柱分离,采用超高效液相色谱分析,内标法定量。结果该测定化妆品中7种激素的方法在一定范围内线性良好(r>0.995),己烯雌酚和丙酸睾丸素的线性范围为0.1μg/ml~5.0μg/ml,其余5种激素的线性范围为0.2μg/ml~5.0μg/ml;最低检出浓度为0.02μg/g~0.04μg/g,平均回收率为80.1%~95.8%,相对标准偏差为2.1%~7.2%。结论该方法操作简便、灵敏度高,适用于化妆品中7种激素的快速准确测定。

Objective The solid-phase micro extraction conditions were optimized by the combination of single factor change and response surface optimization methodology,and the solid-phase micro extraction(SPME)-ultra performance liquid chromatography method(UPLC) was established for the determination of seven hormones in cosmetics,including clobetasol propionate,diethylstilbestrol,β-estradiol,ethinylestradiol,progesterone,norgestrel and testosterone propionate.Methods After the sample was ultrasonically extracted with acetonitrile solution,the sample extract was directly extracted with 85 μm PA extraction head at 60 °C and 600 r/min for 50 min,and then desorbed in acetonitrile for 5 min.The desorbed solution was separated by C18 liquid chromatography column for ultra-performance liquid chromatography(UPLC) analysis and quantified by internal standard method.Results The linearity of seven hormones in cosmetics was good within a certain range(r>0.995),and the linear ranges of diethylstilbestrol and testosterone propionate were within 0.1 μg/ml-5.0 μg/ml,while those of the other five hormones were within 0.2 μg/ml-5.0 μg/ml.The minimum detectable concentration was within 0.02 μg/g-0.04 μg/g.The average recoveries were from 80.1% to 95.8%,and the relative standard deviation(RSD) was within2.1%-7.2%.Conclusion This method is simple and sensitive,and suitable for rapid and accurate detection of 7 hormones in cosmetics.