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

J Agric Food Chem. 2021 Jun 16;69(23):6676-6689. doi: 10.1021/acs.jafc.0c05950. Epub 2021 Jun 8.

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.

Keywords: UPLC−MS/MS; breast milk; extraction; nonpersistent pesticides; simple.

MeSH terms

  • Chromatography, High Pressure Liquid
  • Chromatography, Liquid
  • Female
  • Humans
  • Milk, Human / chemistry
  • Pesticides* / analysis
  • Reproducibility of Results
  • Solid Phase Extraction
  • Tandem Mass Spectrometry*

Substances

  • Pesticides