Rapid determination of thirteen organophosphorus flame retardants in milk by using modified Quick, Easy, Cheap, Effective, Rugged, and Safe technique, solid-phase extraction and HPLC-MS/MS.

Abstract

Organophosphorus flame retardants are a class of widely used plasticizers and flame retardants. In this study, an analytical methodology for the simultaneous determination of thirteen organophosphorus flame retardants in milk was developed by using HPLC-MS/MS in combination with a modified quick, easy, cheap, effective, rugged, and safe technique and solid-phase extraction. The experimental parameters of the sample purification procedure and HPLC-MS/MS were optimized. The developed method was validated in terms of linearity, limits of detection, recovery and precision. The method showed a linear response in the 1-100 ng/mL concentration range, and the limits of detection ranged from 0.001 to 0.3 ng/mL. The mean recoveries for most organophosphorus flame retardants were in the ranges of 75.0-115.8% (spiked at 2.5 ng/mL) and 76.7-124.8% (spiked at 25 ng/mL), with relative standard deviations of less than 13.09%. The developed methodology was successfully applied to the analysis of 9 human milk samples and 9 commercial cow milk samples. Eleven organophosphorus flame retardants were detected in the human milk samples, with median concentrations that ranged from lower than the limit of detection to 1.47 ng/mL, and only 9 OPFRs were detected in cow milk samples, with median levels of less than 0.32 ng/mL. This article is protected by copyright. All rights reserved.