Quantification of Nonpersistent Pesticides in Small Volumes of Human Breast Milk with Ultrahigh Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry.

Abstract

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.