Method for Determination of Pentobarbital in Dry Dog Food by Gas Chromatography/Mass Spectrometry

A procedure has been developed and validated for measuring the concentration of pentobarbital residues in dry, extruded animal feed in the range of 3−200 ng/g (ppb) with an estimated limit of quantitation of 2 ppb. The method was developed for surveillance purposes:  to measure the concentration of...

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Bibliographic Details
Published in:Journal of agricultural and food chemistry 2001-10, Vol.49 (10), p.4597-4602
Main Authors: Heller, David N, Lewis, Kristin M, Cui, Wei
Format: Article
Language:English
Subjects:
Animal Feed - analysis
Animals
Biological and medical sciences
Biological Products
Dogs
Euthanasia - veterinary
Feed and pet food industries
Food Analysis - methods
Food industries
Fundamental and applied biological sciences. Psychology
Gas Chromatography-Mass Spectrometry - methods
General aspects
Meat
Methods of analysis, processing and quality control, regulation, standards
Minerals
Pentobarbital - analysis
Sensitivity and Specificity
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Summary:A procedure has been developed and validated for measuring the concentration of pentobarbital residues in dry, extruded animal feed in the range of 3−200 ng/g (ppb) with an estimated limit of quantitation of 2 ppb. The method was developed for surveillance purposes:  to measure the concentration of euthanizing agent which might be present in feeds incorporating rendered products which themselves might include some fraction of euthanized animals. A previously published qualitative procedure was modified by adding isotopically labelled pentobarbital as an internal standard. Dry feed was ground and extracted with methanol. The extract was loaded on a mixed-mode (C-18, anion exchange) solid-phase extraction cartridge designed for barbiturate residues. Pentobarbital was eluted and derivatized for gas chromatography/mass spectrometry in positive ion chemical ionization mode. Quantitation was based on the ratio of dimethyl-pentobarbital MH+ (m/z 255) vs dimethyl-pentobarbital-d 5 (m/z 260) in standards and extracts. Accuracy ranged from 112% at 3 ppb to 96% at 200 ppb, with relative standard deviations ranging from 4% at 3 ppb to 2% at 200 ppb. Keywords: Pentobarbital; quantitation; gas chromatography/mass spectrometry; feed; euthanasia
ISSN:0021-8561
1520-5118
DOI:10.1021/jf0106188