建立了超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用（ UPLC-LTQ/Orbitrap MS）快速筛查、定性识别化妆品中24种激素的分析方法。不同剂型的化妆品样品经甲醇超声提取，用 Waters ACQUITY UPLC BEH C18色谱柱（50 mm×2.1 mm，1.7μm）分离，以乙腈和0.1％（v/v）甲酸水溶液为流动相进行梯度洗脱。通过静电场轨道阱全扫描得到激素化合物的准分子离子的精确质量数，实现对化妆品中激素的快速筛查；再以保留时间和数据依赖扫描（ data dependent scan）模式获得的子离子质谱图进行定性确证。24种激素化合物的质量准确度误差小于3×10-6（3 ppm）；线性良好，相关系数大于0.99；检出限≤10μg/kg（S/N=3），能满足实际化妆品样品的分析要求。应用该方法对不同剂型的50余种化妆品样品进行筛查分析，结果良好。该方法是化妆品中激素快速筛查、定性识别的有效方法。
A method of ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry( UPLC-LTQ/Orbitrap MS)was established to screen and con-firm 24 hormones in cosmetics. Various cosmetic samples were extracted with methanol. The extract was loaded onto a Waters ACQUITY UPLC BEH C18 column(50 mm×2. 1 mm,1. 7 μm) using a gradient elution of acetonitrile/water containing 0. 1%( v/v )formic acid for the separa-tion. The accurate mass of quasi-molecular ion was acquired by full scanning of electrostatic field orbitrap. The rapid screening was carried out by the accurate mass of quasi-molecular ion. The confirmation analysis for targeted compounds was performed with the retention time and qualita-tive fragments obtained by data dependent scan mode. Under the optimal conditions,the 24 hor-mones were routinely detected with mass accuracy error below 3×10-6(3 ppm),and good lineari-ties were obtained in their respective linear ranges with correlation coefficients higher than 0. 99. The LODs( S/N=3)of the 24 compounds were ≤10μg/kg,which can meet the requirements for the actual screening of cosmetic samples. The developed method was applied to screen the hor-mones in 50 cosmetic samples. The results demonstrate that the method is a useful tool for the rapid screening and identification of the hormones in cosmetics.
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