scholarly journals Evaluation Of QuEChERS Sample Preparation For Determination Of Benzimidazoles Residues In Meat By UPLC-MS/MS

2021 ◽  
Vol 16 (1) ◽  
pp. 32-40
Author(s):  
O.V. Bayer ◽  
O.V. Bondarets ◽  
V.М. Mykhalska ◽  
L.V. Shevchenko ◽  
О.М. Stupak ◽  
...  

A liquid chromatographic-tandem mass spectrometric (LC–MS/MS) multi-residue method has been used for the simultaneous quantification and identification of 9 residues and metabolites of benzimidazole derivatives that the most widely used as anthelmintic veterinary drugs of animals. The modified QuEChERS method was used for sample preparation, which was initially developed for pesticide residue analysis. This paper highlights how quick, easy, cheap, effective and rugged the QuEChERS extraction method is. The method was successfully validated according to the 2002/657/EC guidelines. Recovery of analytes was in the range 99 – 110 %. The decission limits (ССα ) were calculated at MRL level for analytes with an established permitted limit as next: 104.5 μg kg-1 (albendazole), 53.2 μg kg-1 (fenbendazole), 54.2 μg kg-1 (flubendazole), 12.1 μg kg-1 (levamisole), 53.9 μg kg-1 (cambendazole), 64.2 μg kg-1 (mebendazole), 52.5 μg kg-1 (parabendazole), 105.8 μg kg-1 (thiabendazole), 234.2 μg kg-1 (triclobendazole). The suitability of the assay has been assessed through InterVal Software by quo data GmbH (Germany). The method achieves high quality of the results, good recovery, repeatabilities, within-lab reproducibilities, and wide analytical scope and has practical benefits, low cost, high sample throughput, little labor used and few lab ware.

Foods ◽  
2019 ◽  
Vol 8 (3) ◽  
pp. 101 ◽  
Author(s):  
Slávka Nagyová ◽  
Peter Tölgyessy

A rapid method is proposed for the determination of selected H2SO4 stable organic compounds—eight organochlorines (OCs; hexachloro-1,3-butadiene, pentachlorobenzene, hexachlorobenzene, hexachlorocyclohexane—HCH—isomers, heptachlor) and six polybrominated diphenyl ethers (PBDEs; BDE-28, 47, 99, 100, 153, 154)—in fish samples. In the method, a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation using pH-tuned dispersive liquid–liquid microextraction (DLLME) and H2SO4 digestion fish extract clean-up is followed by gas chromatography–triple quadrupole tandem mass spectrometry (GC–QqQ-MS/MS) analysis. The method was validated in terms of linearity, limits of the method, recovery, accuracy, analysis of standard reference material (NIST SRM 1946), and estimation of combined uncertainty of the measurement (top-down approach). For validation, chub composite samples were used, and subsequently, the method was successfully applied to analysis of real samples of eight fish species. Finally, the method passed the analytical Eco-Scale evaluation as “an acceptable green analysis method”, and showed its advantages (simplicity, rapidity, low cost, high extract clean-up efficiency, good sensitivity) when compared to other reported QuEChERS based methods.


2019 ◽  
Vol 92 (3) ◽  
pp. 419-428
Author(s):  
Maja Pelajić ◽  
Izidor Pelajić ◽  
Dragana Mutavdžić Pavlović ◽  
Dubravka Vitali Čepo

This work reports a new selective and accurate multiresidue procedure for determination of 25 pesticides in red wine by GC-MS. Proposed procedure uses an original approach in sample preparation technique based on QuEChERS theory. Main focus of method development was modification of salts thus increasing ionic strength of solution which improved pesticides partitioning and extraction efficiency. LOQs were in the range 0.01–250 μg L–1 with 56 % of target pesticides below or equal to 10 μg L–1. RSD for most pesticides was < 20 % and recoveries were in the range 70–120 %. Matrix effect was found to be high for five pesticides confirming sample preparation procedure to be efficient. The proposed procedure was applied to 12 wine samples of different variety with determination of 40 % of target pesticides. Developed GC-MS methodology provides novel, selective and accurate approach for determination of 25 pesticide residues in red wine.


2016 ◽  
Vol 99 (6) ◽  
pp. 1403-1414 ◽  
Author(s):  
Klaudia Pszczolińska ◽  
Monika Michel

Abstract Soil samples are complex matrixes; therefore, soil sample preparation is a critical step, and one that is usually expensive, time-consuming, and labor intensive. The quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, originally developed for the determination of pesticides in fruits and vegetables, has been recently modified and adopted for the analysis of pesticides in soil. This paper reviews all aspects of sample preparation, including extraction and clean-up, and describes the applications of conventional and modified QuEChERS techniques. It also presents a comparison of the QuEChERS method with other methods used for sample preparation for determination of pesticides in soil.


2018 ◽  
Vol 16 (1) ◽  
pp. 81-93
Author(s):  
MDH Prodhan ◽  
SN Alam

Determination of organochlorine pesticide residues in shrimp is very important to ensure the consumer’s safety and to fulfill the importer’s demand. Therefore, a simple and efficient multiple organochlorine pesticide residues analytical method using quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction technique and Gas Chromatography coupled with Electron Capture Detector (ECD) has been developed and validated for the determination of 19 organochlorine pesticides (α- BHC, δ- BHC, β- BHC, γ- BHC, Heptachlor, Aldrin, Heptachlor Epoxide, γ- Chlordane, α- Chlordane, α- Endosulfan, 4,4 DDE, Dieldrin, Endrin, 4,4 DDD, β- Endosulfan, 4,4 DDT, Endosulfan sulphate, Methoxychlor, and Endrin Ketone) in shrimp. The method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD) and limit of quantification (LOQ). The average recoveries of the selected pesticides ranged from 84% to 106% with RSDr ≤ 14% in four fortification levels of 0.05, 0.1, 0.2 and 0.3 mg kg-1. The linearity was ≥ 0.996 for all of the selected pesticides with matrix matched calibration standards. The LOD ranged from 0.003 to 0.009 mg kg-1 and the LOQ was 0.05 mg kg-1. This method was applied successfully for the residue analysis of 40 shrimp samples collected from different regions in Bangladesh.SAARC J. Agri., 16(1): 81-93 (2018)


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