Song Dongning, Liu Jing, Liu Yang
National Institutes for Food and Drug Control, Beijing 102629, China.
NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs, Beijing 102629, China.
Molecules. 2023 Jul 27;28(15):5675. doi: 10.3390/molecules28155675.
Rapid detection of harmful estrogens in cosmetics is essential in protecting public health. To reduce time-consuming pretreatment and analytical procedures, a novel reactive paper spray ionization mass spectrometry (RPSI-MS) methodology was developed. RPSI-MS is suitable for quantitatively analyzing estrogens in cosmetics by utilizing an online derivatization reaction between estrogens and 2-fluoro-1-methyl-pyridinium-p-toluene-sulfonate (FluMP). Using estradiol valerate as the internal standard (I.S.), three estrogens, estradiol, estriol, and ethinyloestradiol, in cosmetics were quantitatively characterized within minutes. Multiple parameters were optimized including FluMP concentration and volume, triethylamine amount as well as the drying time. The three estrogens displayed good linearity ranging from 0.002 to 1 μg/mL, with R above 0.99. The recovery results of all the estrogens were within 80~111%. The limit of detection (LOD) was 0.001 μg/mL for the three estrogens. Compared to conventional paper spray ionization mass spectrometry (PSI-MS), extraction is not required and the detection sensitivity of RPSI-MS was improved by 34,000, 80,000, and 1400 times for estradiol, estriol, and ethinyloestradiol, respectively. The protocol established in this paper is sensitive, eco-friendly, and suitable for rapid testing of estrogens in cosmetics.
快速检测化妆品中的有害雌激素对于保护公众健康至关重要。为了减少耗时的预处理和分析程序，开发了一种新型的反应性纸喷雾电离质谱（RPSI-MS）方法。RPSI-MS通过利用雌激素与2-氟-1-甲基吡啶对甲苯磺酸盐（FluMP）之间的在线衍生化反应，适用于定量分析化妆品中的雌激素。以戊酸雌二醇为内标（I.S.），在数分钟内对化妆品中的三种雌激素，即雌二醇、雌三醇和炔雌醇进行了定量表征。对多个参数进行了优化，包括FluMP浓度和体积以及三乙胺用量和干燥时间。这三种雌激素在0.002至1μg/mL范围内显示出良好的线性，相关系数R大于0.99。所有雌激素的回收率在80%至111%之间。三种雌激素的检测限（LOD）均为0.001μg/mL。与传统的纸喷雾电离质谱（PSI-MS）相比，RPSI-MS无需萃取，对于雌二醇、雌三醇和炔雌醇，其检测灵敏度分别提高了34000倍、80000倍和1400倍。本文建立的方法灵敏、环保，适用于化妆品中雌激素的快速检测。
