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Mottier:
J
ournal of
AOAC I
nternational
V
ol.
98, N
o
. 4, 2015
1127
OFFICIAL METHODS
[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.
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
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
246