GB 5009.253-2016_English: PDF (GB5009.253-2016)
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National Food Safety Standard -- Determination of Perfluorooctane Sulfonate (PFOS) and Perfluorooctanoic Acid (PFOA) in Animal-derived Food
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GB 5009.253-2016
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Standards related to: GB 5009.253-2016
| Standard ID | GB 5009.253-2016 (GB5009.253-2016) | | Description (Translated English) | National Food Safety Standard -- Determination of Perfluorooctane Sulfonate (PFOS) and Perfluorooctanoic Acid (PFOA) in Animal-derived Food | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Word Count Estimation | 8,894 | | Date of Issue | 2016-08-31 | | Date of Implementation | 2017-03-01 | | Regulation (derived from) | Announcement of the State Administration of Public Health and Family Planning 2016 No.11 | GB 5009.253-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Standard for Food Safety -
Determination of Perfluorooctane Sulfonate (PFOS) and
Perfluorooctanoic Acid (PFOA) in Animal-derived Food
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. MARCH 1, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China
Table of Contents
1 Scope ... 3
2 Principle ... 3
3 Reagents and Materials ... 3
4 Instruments and Equipment ... 5
5 Preparation of Samples ... 5
6 Analytical Procedures ... 5
7 Mass Control ... 7
8 Expression of Analysis Results ... 8
9 Precision ... 8
10 Others ... 8
Appendix A Mass Spectrometry Reference Conditions ... 10
Appendix B Typical Liquid Chromatography of PFOA and PFOS and the
Internal Standard – Tandem Mass Spectrometry MRM Figure ... 11
National Standard for Food Safety -
Determination of Perfluorooctane Sulfonate (PFOS) and
Perfluorooctanoic Acid (PFOA) in Animal-derived Food
1 Scope
This Standard specifies the method of isotope dilution liquid chromatography-tandem
mass spectrometry in the determination of PFOS and PFOA in animal-derived food.
This Standard shall be applicable to the determination of PFOS and PFOA in
animal-derived food.
2 Principle
Adopt acetonitrile to extract PFOS and PFOA from the sample. Start dispersive solid
phase extraction and purification; adopt liquid chromatography-tandem mass
spectrometer to determine PFOS and PFOA. Adopt the internal standard method to
quantify the content.
3 Reagents and Materials
Unless otherwise indicated, the reagents adopted under this method are of analytical
purity. The water is first-grade water as specified in GB/T 6682.
3.1 Methanol (CH3OH). chromatographic purity.
3.2 Acetonitrile (CH3CN). chromatographic purity.
3.3 Hydrochloric acid (HCl).
3.4 Sodium chloride (NaCl).
3.5 Ammonium acetate (CH3COONH4). chromatographic purity.
3.6 N-propyl ethylenediamine solid phase adsorbent (PSA). 40 μm~60 μm, ProElut
filler, or equivalent.
3.7 C18 absorbent. 40 μm~60 μm, ProElut filler, or equivalent.
3.8 Graphitized carbon black adsorbent (GCB). 40 μm~60 μm, ProElut filler, or
mixed series of standard working fluid of PFOA (density. 0.05 μg/L, 0.1 μg/L, 0.5 μg/L,
1.0 μg/L, 2.0 μg/L, 10.0 μg/L) and mixed series of standard working fluid of PFOS
(density. 0.1 μg/L, 0.2 μg/L, 1.0 μg/L, 10.0 μg/L, 20.0 μg/L, 40.0 μg/L). Prepare mixed
series of standard working solution of 13C4-PFOA (density. 1.0 μg/L) and 1, 2, 3,
4-13C4-PFOS (density. 5.0 μg/L) that contains 13C isotope. Store under the
temperature of -4°C. It can remain valid for 2 months.
4 Instruments and Equipment
4.1 Liquid chromatography-tandem mass spectrometer. equipped with ESI source.
4.2 Nitrogen blowing instrument.
4.3 Grinder.
4.4 Centrifuge, speed≥5,000 r/min.
4.5 Homogenizer, reference speed. 3,400 r/min~24,000 r/min.
4.6 Analytical balance. division value. 0.1 mg and 0.01 g.
5 Preparation of Samples
Take edible part (remove the bone and shell) from fish, shrimp, crab, shellfish,
octopus, chicken, pork and beef. Cut into small pieces, then, use grinder to make it
into meat paste; remove eggshell, then, homogenize it; mix up milk for later usage.
Place the sample in the glass sample bottle, seal it, label it; store it under the
temperature of -18°C.
6 Analytical Procedures
6.1 Pre-processing of Samples
6.1.1 Extracting
Weigh-take 5 g (accurate to 0.01 g) of sample (before usage, unfreeze and
homogenize the sample); place it in 50 mL polypropylene centrifuge tube. Add 400 μL
of mixed standard solution II, then, add 5 mL of water. Start 1 min whirlpool mixing,
then, add 10 mL of acetonitrile (3.2) and 30 μL of hydrochloric acid (3.3); shake it for
10 min. Add 2 g of sodium chloride (3.4); shake again for 10 min; centrifuge at 5,000
r/min for 10 min. Remove supernatant acetonitrile solution, then, place it in another
tube. Place the tube in water bath at 45°C, then, blow nitrogen till it is dry. Add 1 mL of
methanol (3.1) to dilute; use injector to inhale 1 mL. Use 0.22 μm organic membrane
to filter it; reserve for determination.
Before usage, conduct blank test on all organic solvents and test vessels adopted in
this Standard. If their base value is higher than the limit of quantitation, re-evaporate
the organic solvents, or replace the test vessels, until the base value is lower than the
limit of quantitation.
8 Expression of Analysis Results
The content of PFOA and PFOS in the sample shall be calculated in accordance with
Formula (1).
Where.
X - The content of PFOA or PFOS in the sample, expressed in (μg/kg);
A - The peak area ratio between PFOA or PFOS chromatographic peak and the
chromatographic peak of corresponding internal standard substance in the test
solution, and PFOA or PFOS density obtained through standard curve line, expressed
in (μg/L);
Ao - The peak area ratio between PFOA or PFOS chromatographic peak and the
chromatographic peak of corresponding internal standard substance in the blank
solution, and PFOA or PFOS density obtained through standard curve line, expressed
in (μg/L);
V - The ultimate constant volume of the test solution, expressed in (mL);
f - Dilution times of the test solution;
m - The mass of the sample, expressed in (g).
The calculation result shall be expressed as the arithmetic mean value of two
independent determination results obtained under repeatability conditions. The result
shall retain two significant figures.
9 Precision
The absolute difference between the two independent determination results obtained
under repeatability conditions shall not exceed 30% of the arithmetic mean value.
10 Others
The detection limit of PFOA is 0.002 μg/kg; the detection limit of PFOS is 0.02 μg/kg.
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