Pedersen Theresa L, Smilowitz Jennifer T, Winter Carl K, Emami Shiva, Schmidt Rebecca J, Bennett Deborah H, Hertz-Picciotto Irva, Taha Ameer Y
Department of Food Science and Technology, College of Agriculture and Environmental Sciences, University of California-Davis, Davis 95616, California, United States.
Foods for Health Institute, University of California-Davis, Davis 95616, California, United States.
J Agric Food Chem. 2021 Jun 16;69(23):6676-6689. doi: 10.1021/acs.jafc.0c05950. Epub 2021 Jun 8.
Existing methods for the analysis of pesticides in human breast milk involve multiple extraction steps requiring large sample and solvent volumes, which can be a major obstacle in large epidemiologic studies. Here, we developed a simple, low-volume method for extracting organophosphates, pyrethroids, carbamates, atrazine, and imidacloprid from 100 to 200 μL of human breast milk. Multiple extraction protocols were tested including microwave-assisted acid/base digestion and double-solvent extraction with 2 or 20 mL of 2:1 (v/v) dichloromethane/hexane, with or without subsequent solid-phase extraction (SPE) cleanup. Samples were analyzed by liquid chromatography tandem mass spectrometry. Analyte recoveries and reproducibility were highest when 100-200 μL of milk were extracted with 2 mL of dichloromethane/hexane without subsequent SPE steps. Analysis of 79 breast milk samples using this method revealed the presence of carbamates, organophosphates, pyrethroids, and imidacloprid at detection frequencies of 79-96, 53-90, 1-7, and 61%, respectively. This study demonstrates the feasibility of a simple low-volume extraction method for measuring pesticides in human breast milk.
现有的分析人母乳中农药的方法涉及多个提取步骤，需要大量的样品和溶剂，这可能是大型流行病学研究中的一个主要障碍。在此，我们开发了一种简单的小体积方法，用于从100至200μL人母乳中提取有机磷、拟除虫菊酯、氨基甲酸酯、阿特拉津和吡虫啉。测试了多种提取方案，包括微波辅助酸碱消解以及用2或20 mL 2:1（v/v）二氯甲烷/己烷进行双溶剂提取，有无后续固相萃取（SPE）净化。样品通过液相色谱串联质谱法进行分析。当用2 mL二氯甲烷/己烷提取100 - 200μL牛奶且无后续SPE步骤时，分析物回收率和重现性最高。使用该方法对79份母乳样品进行分析，结果显示氨基甲酸酯、有机磷、拟除虫菊酯和吡虫啉的检出频率分别为79 - 96%、53 - 90%、1 - 7%和61%。本研究证明了一种简单的小体积提取方法用于测定人母乳中农药的可行性。
