在线净化液相色谱-高分辨质谱法快速测定化妆品中糖皮质激素

Rapid Determination of Glucocorticoids in Cosmetics by Online Cleanup Liquid Chromatography-High Resolution Mass Spectrometry

基于在线净化液相色谱-四极杆/静电场轨道阱高分辨质谱技术建立了化妆品中41种糖皮质激素的分析方法。样品采用乙腈提取,经Cyclone P在线净化柱净化后,将富集的分析物洗脱转至C18分析柱,经色谱分离后,采用四极杆/静电场轨道阱高分辨质谱以Full Scan/dd MS2模式进行检测。41种化合物在1~100 ng/m L范围内线性良好,相关系数均大于0.992,方法的定量下限(LOQ)为10μg/kg,加标回收率为71.3%~108.5%;相对标准偏差(RSD)为2.7%~7.9%。该方法简化了样品前处理过程,操作简单、快速、高效,适用于化妆品中糖皮质激素的快速筛查和测定。

A new method for rapid determination of 41 glucocorticoids in cosmetics was established by online cleanup liquid chromatography-high resolution quadropole/electrostatic field orbitrap mass spectrometry(HRMS). The sample was extracted with acetonitrile, and purified on a Cyclone P column. The enriched analytes were eluted from the extraction column and transferred into a C18 analytical column, then analyzed by HRMS in Full Scan/ddMS2 mode. The 41 glucocorticoids showed good linear relationships in the range of 1 to 100 ng/mL, the correlation coefficient were greater than 0.992. The lower limit of quantitation(LOQ) of the method was 10 μg/kg and the recoveries ranged from 71.3% to 108.5% with relative standard deviations(RSDs) of 2.7% to 7.9%. This method is simple, rapid and efficient, and suitable for rapid screening and determination of glucocorticoids in cosmetics.