Rapid determination of 13 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 13 organophosphorus flame retardants in milk was developed by using high‐performance liquid chromatography‐tandem mass spectrometry 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 high‐performance liquid chromatography‐tandem mass spectrometry 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 <13.09%. The developed methodology was successfully applied to the analysis of nine human milk samples and nine 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 nine organophosphorus flame retardants were detected in cow milk samples, with median levels of <0.32 ng/mL.

Occurrence and Dietary Intake of Organophosphate Esters via Animal-Origin Food Consumption in China: Results of a Chinese Total Diet Study

“…Food samples were analyzed according to our previous study. , Briefly, a modified Quick, Easy, Cheap, Effective, Rugged, and Safe technique (QuEChERS) coupled to solid-phase extraction was used for sample pretreatment. Quantitative analysis was carried out by an Acquity HPLC (Waters, MA) coupled with an electrospray triple quadrupole mass spectrometry system (Micromass Xevo TQS, Waters, MA).…”

Method validation and residue analysis of methoxyfenozide and metaflumizone in Chinese broccoli under field conditions by liquid chromatography with tandem mass spectrometry

“…It has been reported that a wide range of compounds with different polarities could be extracted by acetonitrile with a few lipophilic co-extracts such as lipid and pigments [30,31]. The extraction efficiency and stability of some acidic and base-sensitive pesticides could be improved by properly increasing the acidity of extraction solvent [32].…”

Determination of organophosphate flame retardant tris(2‐chloroethyl)phosphine based on the luminol–H2O2 chemiluminescence system

“…[18] Most existing methods for detecting TCEP involve gas chromatography and mass spectrometry (GC/MS), [19] as well as liquid chromatography and mass spectrometry (LC/MS). [20] Although these methods have relatively high reliability, they also have many disadvantages that cannot be ignored, such as long preprocessing time, slow analysis speed, high cost and so on, and therefore these have not been widely used.…”