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Joseph et al.:
J
ournal of
AOAC I
nternational
V
ol.
98, N
o
. 3, 2015
1121
(The method has been validated in cow, goat, and sheep dairy
powders, and dairy powder formulations. It can be used for
other similar matrixes, including liquid milk, provided that it
is demonstrated that the method performance values are met.)
Specific hazards
.—
Hydrochloric acid
.—Wear personal
protective equipment (PPE) and handle in a fume cupboard.
Sulfuric acid
.—Wear PPE and handle in a fume cupboard.
Sodium fluoroacetate
.—Wear PPE, including safety glasses
and a dust mask, when weighing out the primary material.
Potassium hydroxide
.—Wear PPE and handle in a fume
cupboard; avoid inhalation of dust.
3-Nitroaniline
.—Wear PPE, including safety glasses; avoid
inhalation.
Phosphoric acid
.—Wear PPE and handle in a fume cupboard.
Sodium fluoroacetate (Figure
2015.02A
) is a rodenticide
used in New Zealand to control rats, possums, and rabbits.
It is commonly known by its original registration number
as compound 1080, but may also be known as sodium
monofluoroacetate and fluoroacetic acid sodium salt.
A. Principle
Samples are dissolved in water and extracted into acetone
to allow precipitation of proteins. After centrifugation, the
solutions are passed through an anion exchange column and
eluted with acid to give free fluoroacetic acid. This acid is
converted to 2-fluoro-3’-nitroacetanilide via a carbodiimide-
mediated amide coupling reaction. The derivative is then
subjected to SPE cleanup, eluting with
t
-butyl methyl ether
(TBME)–
n
-hexane, concentrated and quantified by LC-MS/MS
using derivatized isotopically substituted sodium fluoroacetate
as an internal standard. The method reports the analyte as
fluoroacetic acid.
B. Apparatus
Note
: Where specific equipment is listed, other brands
or models may be used provided that they have equivalent
performance.
Laboratory equipment
.—
(
a
)
Air displacement pipets.—
5000 μL, with long tips.
(
b
)
Autosampler vials
.—2 mL with tapered glass inserts.
(
c
)
Balance
.—2 or 3 decimal top pan.
(
d
)
Balance
.—5 decimal place analytical.
(
e
)
Centrifuge
.—Capable of centrifuging 15 and 50 mL
tubes at 4200 ×
g
RCF.
(
f
)
Centrifuge tubes
.—15 and 50 mL, tapered polypropylene.
(
g
)
Extraction cartridges
.—Oasis HLB 60 mg.
(
h
)
Glass reservoirs
.— Ground glass, 19/26 joint,
approximately 20 mL.
Determination of Sodium Monofluoroacetate in Dairy
Powders by Liquid Chromatography Tandem Mass
Spectrometry (LC-MS/MS): First Action 2015.02
George Joseph
AssureQuality, Blockhouse Bay, 131 Boundary Rd, Lynfield, Auckland 0600, New Zealand
Submitted for publication April 2015.
Adopted as a First Action Official Method by the Expert Review
Panel on Sodium Monofluoroacetate and approved by the Stakeholder
Panel on Infant Formula and Adult Nutritionals (SPIFAN).
Approved on: March 17, 2015.
DOI: 10.5740/jaoac.int.2015.02
OFFICIAL METHODS
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
240