Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review

Recent developments and applications of QuEChERS based techniques on food samples during pesticide analysis

Recent progress in immunosensors for pesticides

A QuEChERS extraction followed by GC/MS/MS and GC-μECD/NPD for 216 pesticide and metabolites determination in soil simultaneously were developed and compared. Volume of water, volume and polarity of solvent, and cleanup sorbents (C18, GCB, PSA) were optimized. The QuEChERS with and without purification step were applied to estimate effectiveness of the method. The recovery and matrix effect (ME) were critical parameters within each tested procedure. The optimal method without cleanup was validated. Accuracy (expressed as recovery), precision (expressed as RSD), linearity, LOQ, and uncertainty were determined. The recoveries at the three spiking levels using matrix-matched standards ranged between 65 and 116% with RSD ≤17 and 60-112% with RSD ≤18% for MS/MS and μEC/NP, respectively. The LOQ ranged from 0.005-0.01 mg/kg for MS/MS to 0.05 mg/kg for μEC/NP. The ME for most of pesticides resulted in enhancement of the signal and depended on the analyte and detection system: MS/MS showed ME from -25 to 74%, while μEC/NP from -45 to 96%. A principal component analysis was performed to explain the relationships between physicochemical parameters and ME of 216 pesticides. The QuEChERS protocol without the cleanup step is a promising option to make the method less expensive and faster. This methodology was applied in routine analysis of 263 soil samples in which p,p' DDT was the most frequently detected (23.5% of samples) and pendimethalin with the highest concentration (1.63 mg/kg).

/pdf/influence-of-quechers-modifications-on-recovery-and-matrix-1aitfy1fig.pdf

Influence of QuEChERS modifications on recovery and matrix effect during the multi-residue pesticide analysis in soil by GC/MS/MS and GC/ECD/NPD

An accurate, rapid, and reliable multiresidue QuEChERS method based on gas chromatography coupled with tandem mass spectrometry was developed for the determination of 235 pesticides in challenging, dry, complex herb matrices (Centaurea cyanus L, Matricaria chamomilla L, Thymus vulgaris L) Sample mass and the type of cleanup sorbent used to estimate the procedure’s effectiveness were optimized Purification steps with ChloroFiltr, ENVI-Carb, GCB, octadecyl, PSA, and Z-Sep as cleanup sorbents and a step without purification were compared To minimize the matrix effect and obtain acceptable recoveries for pesticides, 2 g of herb sample and 10 mL acetonitrile, followed by d-SPE cleanup step with a combination of 150 mg PSA/45 mg ENVI-Carb/900 mg MgSO4, and additionally 50 μL of 5% formic acid and some droplets of dodecane, were needed Matrix effects for the vast majority of pesticides were reduced (> 20%), showing suppression or enhancement Most recoveries were in the range of 70–120% (RSD < 18%), reaching the quantification limit of 0001 to 0002 mg kg−1 There was excellent linearity within the range from 0001 to 200 μg mL−1, and a correlation coefficient higher than 0999 was obtained Expanded measurement uncertainty was estimated to be between 4 and 43% Finally, the developed method was successfully employed to identify and quantify pesticide residues in the analysis of 46 real herb samples

/pdf/modification-of-multiresidue-quechers-protocol-to-minimize-1wimi1025o.pdf

Modification of Multiresidue QuEChERS Protocol to Minimize Matrix Effect and Improve Recoveries for Determination of Pesticide Residues in Dried Herbs Followed by GC-MS/MS

Multiclass pesticide residue analysis in fish muscle and liver on one-step extraction-cleanup strategy coupled with liquid chromatography tandem mass spectrometry

Multi-residue methods for the determination of over four hundred pesticides in solid and liquid high sucrose content matrices by tandem mass spectrometry coupled with gas and liquid chromatograph.

The rapid analytical method was developed in response to increasing concern over the environmental impact of azoles (sterol biosynthesis inhibitors) and neonicotinoids (nicotinic acetylcholine receptor site). These chemicals are commonly used to protect fruit and vegetables crops against fungi and pests. Seven insecticides and twenty one fungicides commonly occurring in food industrial wastewater have been determined. For this purpose, active substances from two new pesticide classes were extracted and isolated by QuEChERS by addition of acetonitrile, buffering salts and chitin as a clean-up sorbent. The novelty of this procedure was one step sample preparation including extraction and removing of co-extracts in short time. Instrumental analysis was conducted by liquid chromatography coupled with mass spectrometry using multiple reaction monitoring. The limits of detection ranged from 0.002 to 0.005 μg·L-1 with satisfactory accuracy and precision The recoveries for the pesticides ranged from 81–103%, with high repeatability (n = 3, RSD ≤ 9%) and low LOQs (0.01 μg·L-1). Matrix effects calculated were less than 12% for all analyses. The method was applied to routine analysis of food industrial wastewater. Concerning the results, total pesticide levels in most cases were below 1 μg·L-1. The most significant pesticides in terms of concentration and frequency of detection were acetamiprid (0.07 μg·L-1); tebuconazole (1.2 μg·L-1) and thiacloprid (0.04 μg·L-1).

/pdf/new-rapid-analysis-of-two-classes-of-pesticides-in-food-be9vq45nxd.pdf

New Rapid Analysis of two Classes of Pesticides in Food Wastewater by Quechers-Liquid Chromatography/Mass Spectrometry

The aim of this study was to develop the multiresidue method for the determination of 426 pesticide residues in root vegetables (beetroot, carrot, parsnip, parsley, radish and celery) based on QuEChERS method extraction. Optimization of the method included selection of the parameters such as a sample weight, extracting solvent and sorbent in a clean-up step. The optimum parameter was the application of 10 g sample weight/10 ml 1% formic acid in acetonitrile/clean-up 150 mg MgSO4 + 25 mg primary secondary amine + 2.5 mg graphitized carbon black. Active substances were determined by gas chromatography and liquid chromatography coupled with tandem quadrupole mass spectrometry (GC-MS/MS and LC-MS/MS). The average recoveries for most compounds were in the range 72.3−119.4% and the relative standard deviations were 0.3−16.2%. The developed method allowing the determination of very low concentration levels (0.005 mg/kg) has been adapted for routine tests defining the pesticide residues in root vegetables. The obtained results were highly satisfactory and demonstrated their compliance with the criteria recommended by the European Union document SANTE/11945/2015.

Optimization of the multiresidue method for the determination of pesticide residues in root vegetablesOptymalizacja wielopozostałościowej metody oznaczania pozostałości pestycydów w warzywach korzeniowych

Julia Szabunko

Papers

Multiclass pesticide residue analysis in fish muscle and liver on one-step extraction-cleanup strategy coupled with liquid chromatography tandem mass spectrometry

Multi-residue methods for the determination of over four hundred pesticides in solid and liquid high sucrose content matrices by tandem mass spectrometry coupled with gas and liquid chromatograph.

New Rapid Analysis of two Classes of Pesticides in Food Wastewater by Quechers-Liquid Chromatography/Mass Spectrometry

Optimization of the multiresidue method for the determination of pesticide residues in root vegetablesOptymalizacja wielopozostałościowej metody oznaczania pozostałości pestycydów w warzywach korzeniowych