Examination of Proficiency and Control Recovery Data from Analyses for Pesticide Residues in Food: Sources of Variability

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We examined a number of large proficiency and control databases supporting the values reported for pesticide residues in agricultural commodities at fractions of a part per million (mg/kg). The average recovery from >100 000 recovery records in 13 databases was 94%. The overall average single-value relative standard deviation (RSD) of the reported recoveries was 17% at a mean concentration (C) of about 10−7 (0.1 mg/kg). The average apparent HORRAT value (RSD found/RSDR predicted from the Horwitz formula [2*C−0.1505]) was 0.8. Analysis of variance indicated that about 60–70% of the variance could not be associated with any particular factor or combination of factors–analyte, commodity, method, laboratory, concentration, database, or their interactions. The most predominant factor, analyte, and its third-order interaction with laboratory and concentration contributed most of the assignable variance. These findings suggested that most of the variability of trace analysis for pesticide residues is “random” in the sense of being inherent and not assignable to specific factor fluctuations.

Document Type: Research Article

Affiliations: 1: U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, HFS-500, Washington, DC 20204; AOAC INTERNATIONAL, 481 N Frederick Ave, Gaithersburg, MD 20877-2417. 2: California Department of Food and Agriculture, Sacramento, CA 95832. 3: U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, Division of Mathematics, HFS-706, Washington, DC 20204.

Publication date: May 1, 2001

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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 The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better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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