化学衍生化和纸喷雾电离质谱法快速检测化妆品中的雌激素。

Rapid Detection of Estrogens in Cosmetics by Chemical Derivatization and Paper-Spray Ionization Mass-Spectrometry.

机构信息

National Institutes for Food and Drug Control, Beijing 102629, China.

NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs, Beijing 102629, China.

出版信息

Molecules. 2023 Jan 23;28(3):1130. doi: 10.3390/molecules28031130.

DOI:10.3390/molecules28031130

PMID:36770794

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9920920/

Abstract

Estrogens in personal care products are harmful to customers. Conventional methods such as HPLC and LC-MS require tedious sample pretreatment and long analytical time. Paper-spray ionization mass spectrometry (PSI-MS) is a powerful tool for the determination of compounds with little time and minimal pretreatment procedures. Since most estrogens show poor responses in PSI-MS, we developed a chemical derivatization and PSI-MS method to determinate three estrogens: estradiol, estriol and ethinyloestradiol with estradiol valerate as the internal standard (I.S.). After derivatization with 2-fluoro-1-methyl-pyridinium-p-toluene-sulfonate, the three estrogens could be quantified in seconds. This method showed good linearity in the range of 0.1~~30 μg·mL, with R > 0.999. Their recovery results were all between 85%~~115%. The limits of detection (LOD) were 0.04 μg·mL, 0.02 μg·mL and 0.02 μg·mL for estradiol, estriol and ethinyloestradiol respectively, which improved around 200, 2000, and 900 times compared to non-derivative PSI-MS. The method could quantitatively determine estrogens in cosmetics.

摘要

个人护理产品中的雌激素对消费者有害。高效液相色谱法（HPLC）和液相色谱-质谱法（LC-MS）等常规方法需要繁琐的样品预处理和较长的分析时间。纸喷雾电离质谱法（PSI-MS）是一种用于测定化合物的强大工具，其分析时间短，预处理步骤最少。由于大多数雌激素在 PSI-MS 中响应较差，我们开发了一种化学衍生化和 PSI-MS 方法来测定三种雌激素：雌二醇、雌三醇和炔雌醇，以雌二醇戊酸酯为内标（IS）。用 2-氟-1-甲基-吡啶𬭩对甲苯磺酸盐衍生化后，三种雌激素可在数秒内定量。该方法在 0.1~~30 μg·mL 的范围内具有良好的线性关系，R > 0.999。它们的回收率均在 85%~~115%之间。雌二醇、雌三醇和炔雌醇的检测限（LOD）分别为 0.04 μg·mL、0.02 μg·mL 和 0.02 μg·mL，与非衍生 PSI-MS 相比，分别提高了约 200、2000 和 900 倍。该方法可定量测定化妆品中的雌激素。