Data verification in the residue laboratory.

Residue analysis frequently presents a challenge to the quality assurance (QA) auditor due to the sheer volume of data to be audited. In the face of multiple boxes of raw data, some process must be defined that assures the scientist and the QA auditor of the quality and integrity of the data. A program that ensures that complete and appropriate verification of data before it reaches the Quality Assurance Unit (QAU) is presented. The "Guidelines for Peer Review of Data" were formulated by the Residue Analysis Business Center at Ricerca, Inc. to accommodate efficient use of review time and to define any uncertainties concerning what are acceptable data. The core of this program centers around five elements: Study initiation (definitional) meetings, calculations, verification, approval, and the use of a verification checklist.

Multiresidue gas chromatographic method for determining organochlorine pesticides in meats: validation study for swine and beef fats.

A validation of a previously studied method for determining organochlorine residues in poultry fat was conducted to extend the usefulness of the method to beef and swine fats. The validation samples consisted of 16 materials all analyzed in duplicate. Fortification levels ranged from 0.02 to 1.2 ppm for alpha-BHC, lindane, cis- and trans-chlordane, octachlor epoxide, o,p'- and p,p'-DDT, p,p'-DDE, p,p'-TDE, hexachlorobenzene, heptachlor epoxide, dieldrin, endrin, methoxychlor, mirex, and toxaphene. The average recovery was 101% with a range of 79-113%, not including toxaphene. The ranges of coefficients of variation were CVo = 0-23.37% and CVx = 3.74-26.19%. The results were comparable to the previous collaborative study of the same method for poultry fat. The extended method has been adopted official first action.

Multiresidue gas chromatographic method for determining organochlorine pesticides in poultry fat: collaborative study.

A gas chromatographic electron capture detector method is described for the quantitative determination of organochlorine pesticide residues in poultry fat. The samples are rendered and cleaned up using automated gel permeation chromatography. The collaborative samples consisted of 10 fortified samples and one incurred residue sample, all in duplicate. Fortification levels ranged from 0.15 to 1.0 ppm for alpha-BHC, lindane, cis- and trans-chlordane, octachlor epoxide, o,p' and p,p'-DDT, p,p'-DDE, p,p'-TDE, hexachlorobenzene, heptachlor epoxide, dieldrin, endrin, methoxychlor, mirex, and toxaphene. The average recovery was 91.9% with a range of 81-102%. The ranges of coefficients of variation were: CVo = 3.39-14.79%; CVL = 0-16.6%; and CVx = 5.82-19.0%. The results indicate accuracy and precision comparable to other official methodology. The method has been adopted official first action.