High-Throughput Quantification of Monofluoroacetate (1080) in Milk as a Response to an Extortion Threat

As a food defense measure against an extortion threat to poison infant formula with monofluoroacetate, a robust methodology for monofluoroacetate analysis in fluid milk and powdered dairy products was developed and optimized. Critical challenges posed by this situation required that the analytical m...

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Bibliographic Details
Published in:Journal of food protection 2016-02, Vol.79 (2), p.273-281
Main Authors: Cooney, Terry P, Varelis, Peter, Bendall, Justin G
Format: Article
Language:English
Subjects:
Animals
Baby foods
Cattle
Chromatography
Chromatography, High Pressure Liquid - methods
Dairy products
Extortion
Fluoroacetates - analysis
Food contamination & poisoning
Food Contamination - analysis
Food safety
High-Throughput Screening Assays - methods
Infant Formula - chemistry
Liquid chromatography
Mass spectrometry
Milk
Milk - chemistry
Nervous system
Poisoning
Poisons
Scientific imaging
Sensitivity and Specificity
Sodium
Solid Phase Extraction - methods
Tandem Mass Spectrometry - methods
Threats
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Summary:As a food defense measure against an extortion threat to poison infant formula with monofluoroacetate, a robust methodology for monofluoroacetate analysis in fluid milk and powdered dairy products was developed and optimized. Critical challenges posed by this situation required that the analytical methodology provide (i) high specificity, (ii) high throughput capable of analyzing thousands of samples of fluid milk per day, and (iii) trace-level detection of 1 ng/g or lower to achieve the maximum residue limit. Solid-phase extraction-purified acetone extracts of fluid milk were derivatized with aniline, and after ultrahigh-performance liquid chromatography using a Kinetex-C18 column packed with 1.3-μm shell particles, the resulting N-phenyl 2-fluoroacetamide could be determined by liquid chromatography-tandem mass spectrometry in a highly specific manner and with a limit of quantification of 0.5 ng/ml. By using 4-(4-chlorophenoxy)aniline as a derivatizing agent, the method could be extended to powdered dairy products with the same limit of quantification. Between January and July 2015, some 136,000 fluid milk samples were tested using this method. This analytical testing of fluid milk formed one element in a larger program of work by multiple agencies to ensure that consumers could continue to have confidence in the safety of New Zealand milk and dairy products.
ISSN:0362-028X
1944-9097
DOI:10.4315/0362-028X.JFP-15-405