The paper reports the study of gel permeation chromatography (GPC), gas chromatography/mass spectrometry (GS/MS), and column chromatography tandem MS (LC/MS/MS) for 839 pesticides and chemical contaminants, through which a GPC data bank has been established for 744 pesticides, a GC/MS
data bank for 541 pesticides, and an LC/MS/MS data bank for 464 pesticides. On the basis of this study, a new method for quantitative determination of 587 pesticide residues in animal muscles such as beef, mutton, pork, chicken, and rabbit has been established using GPC cleanup followed by
GC/MS and LC/MS/MS. In the method, 10 g animal samples were mixed with 20 g sodium sulfate and extracted twice with 35 mL cyclohexaneethyl acetate (1 + 1) by blender homogenization followed by centrifugation, filtration, and concentration. An equivalent of 5 g sample was injected into a 400
25 mm S-X3 GPC column, with cyclohexaneethyl acetate (1 + 1) as the mobile phase at a flow rate of 5 mL/min. The 2240 min fraction was collected for subsequent analysis. For the 478 pesticides determined by GC/MS, the portions collected from GPC were concentrated to 0.5 mL and exchanged twice
with 5 mL hexane. For the 379 pesticides determined by LC/MS/MS, the portions collected from GPC were dissolved with acetonitrilewater (60 + 40) after taking the extract to dryness with nitrogen gas. At the limit of quantification (LOQ) and 10 LOQ fortification levels of 0.116 000 g/kg, recoveries
were within 40130, among which 563 pesticide recoveries were between 60 and 130, accounting for 96 of the compounds; 24 analytes were recovered between 40 and 60, accounting for 4 of the compounds. The relative standard deviation was below 30 for all 587 pesticides. The limits of detection
for the method were 0.11600 g/kg. In comparison with GC/MS, LC/MS/MS increased the detection sensitivity 21000 times for 236 pesticides.
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Document Type: Research Article
Qinhuangdao Entry-Exit Inspection and Quarantine Bureau, 39 Haibin Rd, Qinhuangdao, Hebei, People's Republic of China.
Shandong Agriculture University, 61 Daizong St, Taian, People's Republic of China.
Publication date: 2009-05-28
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The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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