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Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables.

Journal of chromatography. A (2010-02-11)
Steven J Lehotay, Kyung Ae Son, Hyeyoung Kwon, Urairat Koesukwiwat, Wusheng Fu, Katerina Mastovska, Eunha Hoh, Natchanun Leepipatpiboon
ABSTRACT

This article describes the comparison of different versions of an easy, rapid and low-cost sample preparation approach for the determination of pesticide residues in fruits and vegetables by concurrent use of gas and liquid chromatography (GC and LC) coupled to mass spectrometry (MS) for detection. The sample preparation approach is known as QuEChERS, which stands for "quick, easy, cheap, effective, rugged and safe". The three compared versions were based on the original unbuffered method, which was first published in 2003, and two interlaboratory validated versions: AOAC Official Method 2007.01, which uses acetate buffering, and European Committee for Standardization (CEN) Standard Method EN 15662, which calls for citrate buffering. LC-MS/MS and GC-MS analyses using each method were tested from 50 to 1000ng/g in apple-blueberry sauce, peas and limes spiked with 32 representative pesticides. As expected, the results were excellent (overall average of 98% recoveries with 10% RSD) using all 3 versions, except the unbuffered method gave somewhat lower recoveries for the few pH-dependent pesticides. The different methods worked equally well for all matrices tested with equivalent amounts of matrix co-extractives measured, matrix effects on quantification and chemical noise from matrix in the chromatographic backgrounds. The acetate-buffered version gave higher and more consistent recoveries for pymetrozine than the other versions in all 3 matrices and for thiabendazole in limes. None of the versions consistently worked well for chlorothalonil, folpet or tolylfluanid in peas, but the acetate-buffered method gave better results for screening of those pesticides. Also, due to the recent shortage in acetonitrile (MeCN), ethyl acetate (EtOAc) was evaluated as a substitute solvent in the acetate-buffered QuEChERS version, but it generally led to less clean extracts and lower recoveries of pymetrozine, thiabendazole, acephate, methamidophos, omethoate and dimethoate. In summary, the acetate-buffered version of QuEChERS using MeCN exhibited advantages compared to the other tested methods in the study.

MATERIALS
Product Number
Brand
Product Description

Supelco
Supel QuE, Citrate Extraction Tube, pk of 50, suitable for EN 15662
Supelco
Supel QuE, Acetate Tube, pk of 50, AOAC® 2007.01
Supelco
Supel QuE, PSA Tube, pk of 50, suitable for EN 15662:2008 per BS
Supelco
Supel QuE, PSA Tube, pk of 50, AOAC® 2007.01
Supelco
Supel QuE, PSA/C18/ENVI-Carb Tube, pk of 50, AOAC® 2007.01
Supelco
Supel QuE, PSA Tube, pack of 100, AOAC® 2007.01
Supelco
Supel QuE, PSA/C18 Tube, pack of 100, AOAC® 2007.01
Supelco
Supel QuE, PSA/C18/ENVI-Carb Tube, pack of 100, AOAC® 2007.01
Supelco
Supel QuE, Z-Sep/C18 Tube, centrifuge tube volume 2 mL, pack of 100
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep+ Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, PSA Tube, pack of 50 ea, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/C18 Tube (Shaker Compatible), pk of 50, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/ENVI-Carb Tube 1, pk of 50, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/ENVI-Carb Tube 2, pk of 50, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA Tube, pk of 50, AOAC® 2007.01, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/C18 Tube, pk of 50, AOAC® 2007.01, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/C18/ENVI-Carb Tube, pk of 50, AOAC® 2007.01, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep/C18 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible