6. AOACSPIFANMethods-2018Awards

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Mottier: J ournal of AOAC I nternational V ol. 98, N o . 4, 2015  1127

OFFICIAL METHODS

Determination of Sodium Fluoroacetate in Infant Formula by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS): First Action 2015.03 Pascal Mottier Nestlé Research Center, Nestec Ltd, Analytical Sciences Department, Vers-chez-les-Blanc, PO Box 44, CH-1000 Lausanne 26

Stakeholder Panel on Infant Formula and Adult Nutritionals Expert Review Panel for Working Group for Sodium Fluoroacetate Darryl Sullivan (Chair) , Covance Martin Alewijn , RIKILT John Austad , Covance Joe Boison , CFIA/Univ of Saskatoon Scott Christiansen , Perrigo Jo Marie Cook , Florida State Dept of Agriculture Jon DeVries , Medallion Labs/General Mills Harvey Indyk , Fonterra George Joseph , AsureQuality Erik Konings , Nestle Alex Krynitsky , U.S. Food and Drug Administration Tom Phillips ,Maryland State Dept of Agriculture Bert Popping , Merieux NutriSciences Murali Reddy , Abbott John Wong , U.S. Food and Drug Administration

[Applicable for the quantitative determination of sodium fluoroacetate in liquid and powdered milk- and soy-based infant formulas by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The limit of quantification (LOQ) of sodium fluoroacetate is 1 µg/kg by this method. Application of this method to matrices not covered by the scope of application requires an additional validation.] Caution : Material Safety Data Sheets (MSDS) should be available for all chemicals; inherent risks and corresponding safety precautions shall be identified. Follow general safety precautions and environmental aspects as described in the local Safety, Health and Environment rules in place. Sodium fluoroacetate is highly toxic to humans. Take all necessary precautions, especially when working with concentrated stock standard solutions. Sodium fluoroacetate (Figure 2015.03A ) is a synthetic pesticide known as “1080” and used to fight mammalian pest species. Farmers and graziers use the poison to protect pastures and crops from various herbivorous mammals. It is used as well to protect sheep and goats from predatory coyotes (predacide). In New Zealand and Australia, it is used to control invasive non-native mammals that prey on or compete with native wildlife and vegetation. Sodium fluoroacetate is highly toxic to mammals, including humans. This pesticide is approved for use in the following countries: United States, Canada, Mexico, Australia, New Zealand, Korea, Japan, and Israel. New Zealand has used “1080” for pest control since the 1950s, while the United States began use in the 1940s. Sodium fluoroacetate is also a naturally occurring poison found in at least 40 plants native in Australia, South and West Africa, and Brazil. A. Principle Milk powder is first reconstituted in water. Liquid sample is used as such. Acetonitrile is added to precipitate proteins. After centrifugation, the supernatant is washed with hexane and then acidified with concentrated sulfuric acid. QuEChERS salts (MgSO 4 and NaCl) are added for phase separation and the mixture is centrifuged. The resulting supernatant is evaporated to 0.5 mL remaining volume and centrifuged before LC-MS/MS analysis in selected reaction monitoring (SRM) by electrospray ionization (ESI) in negative mode. The compound is analyzed as its fluoroacetate anion.

Submitted for publication March 2015. Adopted as a First Action Official Method by the Expert Review Panel on Sodium Fluoroacetate (Compound 1080) and approved by the Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN).

Approved on: March 16, 2015. DOI: 10.5740/jaoac.int.2015.03