Multiresidue analysis of 30 organochlorine pesticides in milk and milk powder by gel permeation chromatography-solid phase extraction-gas chromatography-tandem mass spectrometry

Abstract

A method for simultaneous determination of the 30 organochlorine pesticides (OCP) in milk and milk powder samples has been developed. Prior to the gas chromatography-tandem mass spectrometric analysis, the residual OCP in samples were extracted with n-hexane and acetone mixture (1/1, vol/vol) and cleaned up by gel permeation chromatography and solid phase extraction. Selected reaction monitoring mode was used for gas chromatography-tandem mass spectrometric data acquisition to identify and quantify the OCP. To avoid the matrix effects, matrix-matched calibration solutions ranging from 2 to 50 ng/mL were used to record the calibration curve. Limits of quantification of all OCP were 0.8 μg/kg. With the exception of endrin, limits of quantification are significantly lower than maximum residue limits set by the European Union and China. The average recoveries were in the range of 70.1 to 114.7% at 3 spiked concentration levels (0.8, 2.0, and 10.0 μg/kg) with residual standard deviation lower than 12.9%. The developed method was successfully applied to analyze the OCP in commercial milk products.

Determination of 107 Pesticide Residues in Wolfberry with Acetate-buffered Salt Extraction and Sin-QuEChERS Nano Column Purification Coupled with Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

“…In recent years, mass spectrometry (MS) technology has been developing continuously, among which LC coupled with tandem MS (LC-MS/MS) is an effective and sensitive method for the detection of pesticide residues [25,26]. Common sample pretreatment techniques including liquid-liquid extraction (LLE) [27], solid phase extraction (SPE) [28,29], microwave-assisted extraction (MAE) [29,30], supercritical fluid extraction (SFE) [31], accelerated solvent extraction (ASE) [32,33,34], magnetic solid phase extraction (MSPE) [35,36], gel permeation chromatography (GPC) [37,38,39], as well as the QuEChERS method (quick, easy, cheap, effective, rugged and safe) which was firstly published by Anastassiades et al in 2003 [40]. Nowadays, the QuEChERS protocol has been widely used for the determination of pesticide residues due to its significant advantages [41].…”

Impact of DDT residues in feed on thyroid gland and liver secretory activity of Aberdeen-Angus cattle depending on cattle age and sex

“…Milk samples for DDT residues determination were prepared according to Zheng et al (2014), with some modifications. Milk (10 g) was weighed in a 50 ml centrifuge tubes.…”

A Review: Sample Preparation Methods for the Pesticide Residue Analysis in Food Samples

“…A method for simultaneous determination of the organochlorine pesticides in milk and milk powder sample has been developed by gel permeation chromatography-solid phase extraction-gas chromatography-tandem mass spectrometry [6]. Limit of quantification of all organochlorine pesticides were 0.8µg/kg.…”