GB 31604.50-2020 PDF in English
GB 31604.50-2020 (GB31604.50-2020) PDF English
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National food safety standard - Food contact materials and articles - Determination of nonylphenol migration
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Standards related to: GB 31604.50-2020
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GB 31604.50-2020: PDF in English GB 31604.50-2020
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Food contact materials
and articles - Determination of nonylphenol migration
ISSUED ON: SEPTEMBER 11, 2020
IMPLEMENTED ON: MARCH 11, 2021
Issued by: National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope ... 3
2 Principle ... 3
3 Reagents and materials ... 3
4 Instruments and equipment... 5
5 Analysis steps ... 6
6 Expression of analysis results ... 8
7 Precision ... 9
8 Others ... 9
Annex A Reference mass spectrometry conditions ... 10
Annex B MRM chromatogram of nonylphenol standard working solution ... 11
National food safety standard - Food contact materials
and articles - Determination of nonylphenol migration
1 Scope
This Standard specifies the liquid chromatography-mass spectrometry/mass
spectrometry method for nonylphenol migration of food contact materials and
articles.
This Standard is applicable to the determination of nonylphenol of food contact
materials and products with water, 4% (volume fraction) acetic acid solution, 10%
(volume fraction) ethanol solution, 20% (volume fraction) ethanol solution, 50%
(volume fraction) ethanol solution, olive oil , 95% (volume fraction) ethanol
solution as food simulant OR the determination of nonylphenol in the soaking
solution obtained by using 95% (volume fraction) ethanol solution, isooctane
chemical substitute solvent in a migration test.
2 Principle
Take 4% (volume fraction) acetic acid solution as food simulant. In the soaking
solution obtained by migration test, add ammonia to neutralize then determine
the injected sample. Use olive oil as a food simulant. The soaking solution
obtained by migration test is extracted by acetonitrile and purified by n-hexane.
Then determine the injected sample. Use isooctane as a chemical alternative
solvent. The soaking solution obtained by migration test is steamed to dry. Use
methanol to reconstitute. Determine the injected sample. For soaking solutions
obtained from other migration tests, soaking liquids for chemical substitute
solvents, directly determine the injected samples. Nonylphenol in the soaking
solution is determined by liquid chromatography-mass spectrometry/mass
spectrometry. Quantitatively determine by external standard method.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are all analytically
pure, and the water is the grade one water specified in GB/T 6682.
3.1 Reagents
3.1.1 Glacial acetic acid (C2H4O2).
(volume fraction) acetic acid solution to set volume to the graduation of scale.
Obtain standard working solutions of which the mass concentrations are
0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L, 0.20mg/L. Before getting
on the machine, it needs to be processed synchronously with the food simulant
soaking solution in accordance with 5.1.2.1.
3.4.3.2 Oil-based food simulant standard working solution
Respectively and accurately weigh 5.00g (to the nearest of 0.1mg) of olive oil
into 6 stoppered glass centrifuge tubes. Respectively add 0.01mL, 0.02mL,
0.03mL, 0.05mL, 0.10mL, 0.20mL of standard intermediate solution (5mg/L).
Vortex to mix well. Obtain 0.01mg/kg, 0.02mg/kg, 0.03mg/kg, 0.05mg/kg,
0.10mg/kg, 0.20mg/kg standard working solutions. Before getting on the
machine, it needs to be processed synchronously with the food simulant
soaking solution in accordance with 5.1.2.2.
3.4.3.3 Isooctane standard working solution
Respectively and accurately pipette 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL,
0.40mL of standard intermediate solution (5mg/L) into six 10mL volumetric
flasks. Use isooctane to set volume to the graduation of scale. Mix well. Obtain
standard working solutions of which the mass concentrations are 0.01mg/L,
0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L, 0.20mg/L. Before getting on the
machine, it needs to be processed synchronously with the food simulant
soaking solution in accordance with 5.1.2.3.
3.4.3.4 Standard working solutions of other food simulants, chemical
alternative solvents
Respectively pipette 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL, 0.40mL of
standard intermediate solution (5mg/L) into six 10mL volumetric flasks. Use
corresponding food simulants or chemical alternative solvents to set volume to
the graduation of scale. Obtain other water-based food simulants or chemical
alternative solvent standard working solutions of which the mass concentrations
are 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L, 0.20mg/L.
4 Instruments and equipment
4.1 Liquid chromatography tandem triple quadrupole mass spectrometer:
equipped with electrospray ion source (ESI).
4.2 Vortex oscillator.
4.3 Analytical balance: resolutions are 0.0001g, 0.01g.
4.4 High-speed centrifuge: the maximum speed>10000r/min.
5.2 Instrument reference conditions
5.2.1 Liquid chromatography conditions
The reference conditions of liquid chromatography are as follows:
a) Chromatographic column: C18 column, 2.6μm, 2.1mm×150mm (or
equivalent chromatographic column).
b) Mobile phase: methanol-water (90+10, volume ratio).
c) Flow rate: 0.3mL/min.
d) Column temperature: 40°C.
e) Injection volume: 2μL.
5.2.2 Mass spectrometry conditions
The mass spectrometry reference conditions are as follows:
a) Ionization mode: electrospray ionization negative ion mode (ESI-).
b) Mass spectrometry scan mode: multiple reaction monitoring (MRM).
c) For other mass spectrometer parameters, refer to Table A.1 in Annex A.
5.3 Drawing of standard curve
According to the instrument reference conditions listed in 5.2, determine the
standard working solution. Take the concentration of nonylphenol in the
standard working solution as the abscissa, the corresponding quantitative ion
peak area as the ordinate to draw the standard curve and obtain linear equation.
Refer to Annex B for the chromatogram of the nonylphenol standard working
solution.
5.4 Determination of test solution
5.4.1 qualitative determination
According to the instrument reference conditions listed in 5.2, determine the
food simulant test solution and standard working solution. If the deviation of the
retention time of the mass chromatographic peak of the analyte in the test
solution and the standard solution is within ±2.5%, the signal-to-noise ratio of
all qualifier ions exceeds 3:1; the relative abundance of the qualitative ion pair
is consistent with the relative abundance of the standard solution of equivalent
concentration. When the relative abundance deviation does not exceed the
provisions of Table 1, it can be judged that the corresponding analyte exists in
and articles to the volume (V) of food or food simulants; the density of various
liquid foods is usually calculated as 1kg/L, in square decimeters per kilogram
(dm2/kg). When S/V is known in actual use, F is the actual S/V. When S/V
cannot be estimated, F uses 6dm2/kg, that is, 6dm2 of food contact materials
and articles contact 1kg of food or food simulants.
The result retains at least 2 significant digits.
6.2 Calculation of specific nonylphenol migration for food contact
materials and articles of sealed products (expressed in mg/piece)
When the intended use is unknown, when the specific nonylphenol migration
for food contact materials and articels of sealed products is expressed in
mg/piece, it is calculated according to formula (2). The migration test method
used, the contact area of a single sealed product and the food simulant in the
migration test shall be indicated.
Where,
X2 - Specific nonylphenol migration, in milligrams per piece (mg/piece);
n - Quantity of sealing products for immersion, in pieces.
The result retains at least 2 significant digits.
7 Precision
The absolute difference between two independent determination results
obtained under repeatability conditions shall not exceed 10% of their arithmetic
mean.
8 Others
When the S/V in the migration test is the same as the S/V in the actual use
situation, the detection limit of this method for nonylphenol in various food
simulants and chemical alternative solvents is 0.005mg/kg; the limit of
quantification is 0.01mg/kg.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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