IngentaConnect Multi-residue method for the determination of 450 pesticide resid...

Authors: Pang, G.-F.¹; Fan, C.-L.¹; Liu, Y.-M.¹; Cao, Y.-Z.¹; Zhang, J.-J.¹; Fu, B.-L.¹; Li, X.-M.¹; Li, Z.-Y.¹; Wu, Y.-P.¹

Source: Food Additives and Contaminants, Volume 23, Number 8, August 2006 , pp. 777-810(34)

Publisher: Taylor and Francis Ltd

Abstract:

A multi-residue method was developed for the determination of 450 pesticide residues in honey, fruit juice and wine using double-cartridge solid-phase extraction (SPE), gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS-MS). The method development was based on an appraisal of the characteristics of GC-MS and LC-MS-MS for 654 pesticides as well as the efficiency of extraction and purification from honey, fruit juice and wine. Samples were first diluted with water plus acetone, then extracted with portions of dichloromethane. The extracts were concentrated and cleaned up with graphitized carbon black and aminopropyl cartridges stacked in tandem. Pesticides were eluted with acetonitrile+toluene, and the eluates were concentrated. For 383 pesticides, the eluate was extracted with hexane twice and internal standard solution was added prior to GC-MS determination. For 67 pesticides, extraction was with methanol prior to LC-MS-MS determination. The limit of detection for the method was between 1.0 and 300ngg −1 depending on each pesticide analyte. At the three fortification levels of 2.0-3000ngg −1 , the average recovery rates were between 59 and 123%, among which 413 pesticides (92% of the 450) had recovery rates of 70-120% and 35 pesticides (8% of the 450) had recovery rates of 59-70%. There were 437 pesticides (97% of the 450) with a relative standard deviation below 25%; there were 13 varieties (3% of the 450) between 25.0 and 30.4%.

Keywords: Pesticide multi-residue analysis; gas chromatography-mass spectrometry (GC-MS); liquid chromatography-tandem mass spectrometry (LC; honey; fruit juice; wine

Document Type: Research article

DOI: 10.1080/02652030600657997

Affiliations: 1: Qinhuangdao Entry-Exit Inspection and Quarantine Bureau Inspection and Quarantine Technique Centre, No. 39 Haibin Road, Qinhuangdao China Qinhuangdao, 066002 China

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Multi-residue method for the determination of 450 pesticide residues in honey, fruit juice and wine by double-cartridge solid-phase extraction/gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry