Development of a High-Throughput Screening Analysis for 195 Pesticides in Raw Milk by Modified QuEChERS Sample Preparation and Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry

Abstract

This study aimed to develop a simple, high-throughput method based on modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) followed by liquid chromatography quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS) for the rapid determination of multi-class pesticide residues in raw milk. With acidified acetonitrile as the extraction solvent, the raw milk samples were pretreated with the modified QuEChERS method, including extraction, salting-out, freezing, and clean-up processes. The target pesticides were acquired in a positive ion electrospray ionization mode and an All ions MS/MS mode. The developed method was validated, and good performing characteristics were achieved. The screening detection limits (SDL) and limits of quantitation (LOQ) for all the pesticides ranged within 0.1–20 and 0.1–50 μg/kg, respectively. The recoveries of all analytes ranged from 70.0% to 120.0% at three spiked levels (1 × LOQ, 2 × LOQ, and 10 × LOQ), with relative standard deviations less than 20.0%. The coefficient of determination was greater than 0.99 within the calibration linearity range for the detected 195 pesticides. The method proved the simple, rapid, high throughput screening and quantitative analysis of pesticide residues in raw milk.

Molecularly Imprinted Polymeric Sorbent for Targeted Dispersive Solid-Phase Microextraction of Fipronil from Milk Samples

“…Further, for real sample analysis, cow milk was collected to evaluate the effectiveness of MIP for its practical applications. The contamination of cow milk with pesticides through various pathways is becoming inevitable, and that is why a maximum residue limit of various pesticides has been established by the European Commission . In analyses where a targeted detection and quantification of an analyte is required, MIP can be considered superior over other sorbents due to its specific interaction with the analyte.…”

“…The contamination of cow milk with pesticides through various pathways is becoming inevitable, and that is why a maximum residue limit of various pesticides has been established by the European Commission. 41 In analyses where a targeted detection and quantification of an analyte is required, MIP can be considered superior over other sorbents due to its specific interaction with the analyte. Thus, MIP was synthesized to be used as a DSPME sorbent for the targeted determination of fipronil from milk samples.…”

Development and Validation of a Method for Determination of 43 Antimicrobial Drugs in Western-Style Pork Products by UPLC-MS/MS with the Aid of Experimental Design

“…Some interfering substances were extracted together with the target analytes as co-extracts during the extraction process, such as lipids and proteins, which could be removed by using low-temperature precipitation. This method can be simple without using specialized equipment [ 37 ]. Bacon and ham are mainly composed of animal fat and proteins.…”

Recent Advances in the Chromatographic Analysis of Emerging Pollutants in Dairy Milk: A Review (2018–2023)

“…Gas chromatography (GC), utilizing gas as the mobile phase, and liquid chromatography (LC), in which the mobile phase is a liquid, are the most popularly employed types of chromatography for analytical purposes. When combined with different types of detectors, such as mass spectrometers (MSs), ultraviolet detectors (UVs), diode array detectors (DADs), fluorescence detectors (FLDs), flame ionization detectors (FIDs), and electron capture detectors (ECDs), GC and LC play pivotal roles in the analysis, identification, and quantification of a wide variety of contaminants in food and environmental matrices, offering significant efficiency and sensitivity [ 14 , 29 , 30 , 31 ]. Delving into the literature makes it evident that the most commonly employed methods for analyzing and quantifying residual contaminants in milk and dairy products generally rely on chromatographic techniques [ 13 , 32 , 33 , 34 ].…”

“…This extraction process yielded recoveries in the range of 73.4–114.2% for the target antibiotics. The QuEChERS extraction method was chosen for the extraction of different classes of EPs from milk, including pesticides, EDCs, and pharmaceuticals [ 31 , 85 , 86 ].…”