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

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 300 ng g(-1) depending on each pesticide analyte. At the three fortification levels of 2.0-3000 ng g(-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%.

Comparison of Simple and Rapid Extraction Procedures for the Determination of Pesticide Residues in Fruit Juices by Fast Gas Chromatography–Mass Spectrometry

“…Albero et al (2005) developed a multiresidue method for the determination of pesticides using 10 ml juice samples C18cartridge. Pang et al (2006) used graphitized carbon black SPE cartridges in order to extract pesticides from 15 g of fruit juice. An immunoaffinity-based SPE procedure has been also applied for the determination of triazines in fruit juices (Dallüge et al 1999).…”

Development of Analytical Method for the Determination and Identification of Unregistered Pesticides in Domestic for Orange and Brown Rice(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-

“…본 연구에서 gas chromatograph를 이용하여 확립한 분 석법의 신뢰성을 확보하기 위하여 GC/MS에 의한 확인 (confirmation)용 기기분석법을 확립하였다 (Xu et al, 2009;Pang et al, 2006;Alder et al, 2006). GC/MS 분석조건 은 Table 3과 같았다.…”

Modern Extraction Techniques for Pesticide Residues Determination in Plant and Soil Samples

“…As GCB is suitable for removal of lipids, waxes and other nonvolatile, non-polar coextractants with high molecular weight, it is usually used in combination with other sorbent. Thus, Pang et al (2006) used SPE for determination of 446 pesticides in cabbage, tomato, cucumber, spinach, cauliflower, celery, peas, carrots, potatoes, lettuce, onion and leek, and found out that the C18/GCB/-NH2 combination was the best. Except for slightly lower recoveries obtained for onion and leeks, the method was shown as good choice for all other samples.…”