GB 31604.21: Evolution and historical versions
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National food safety standard - Food contact materials and products - Determination of migration of benzoic acid, phthalic acid and trimellitic acid in food
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GB 31604.21-2025
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| GB 31604.21-2016 | English | 85 |
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National food safety standard - Food contact materials and articles - Determination of migration of terephthalic acid
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GB 31604.21-2016
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Basic data | Standard ID | GB 31604.21-2025 (GB31604.21-2025) | | Description (Translated English) | National food safety standard - Food contact materials and products - Determination of migration of benzoic acid, phthalic acid and trimellitic acid in food | | Sector / Industry | National Standard | | Classification of Chinese Standard | C53 | | Word Count Estimation | 11,116 | | Date of Issue | 2025-09-02 | | Issuing agency(ies) | National Health Commission; State Administration for Market Regulation | GB 31604.21-2016: National food safety standard - Food contact materials and articles - Determination of migration of terephthalic acid
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Food contact materials - Polymer - Determiantion of terephthalic acid in food simulants - High performance liquid chromatography
Book People's Republic of China National Standard
National Food Safety Standard
Food contact materials and products
Determination of migration of terephthalic acid
Published 2016-10-19
2017-04-19 implementation
People's Republic of China
National Health and Family Planning Commission issued
Book GB 31604.21-2016
Foreword
Instead of the standard GB/T 23296.10-2009 "food contact materials - Polymer food simulants measured terephthalic acid
HPLC fixed "and SN/T 2184-2008" food contact materials - Polymer food simulants terephthalic acid
High performance liquid chromatography. "
As compared with the present standard GB/T 23296.10-2009 and SN/T 2184-2008, major changes are as follows.
--- standard name was changed to "national food safety standards for food contact materials and products - Determination of terephthalic acid migration";
--- preparing modified food simulant test solution;
--- modify the expression analysis results;
--- modify the limits of detection and quantitation.
National Food Safety Standard
Food contact materials and products
Determination of migration of terephthalic acid
Range 1
This standard specifies a method for determination of acid migration into food contact materials and articles.
This standard is suitable for food contact materials and products Determination of terephthalic acid migration.
Principle 2
Terephthalic acid was separated by high performance liquid chromatography food simulant, UV detector for detection. Water-based, acid,
Alcohol food simulant determined directly by methanol medium was measured olive oil extraction by the food simulant dilute sodium bicarbonate solution. O
Acid as internal standard, using the internal standard method.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are analytically pure water as an aqueous GB/T 6682 provisions.
3.1 Reagent
3.1.1 sodium acetate trihydrate (C2H3O2Na · 3H2O).
3.1.2 sodium bicarbonate (NaHCO3).
3.1.3 heptane (like -C7H16).
3.1.4 methanol (CH3OH). chromatography.
3.1.5 isopropanol (C3H8O).
3.1.6 phosphoric acid (H3PO4).
3.1.7 glacial acetic acid (CH3COOH).
3.1.8 water base, acid, alcohol, oil-based food simulants. the reagents in accordance with a predetermined GB 31604.1.
3.2 Reagent preparation
3.2.1 water base, acid, alcohol, oil-based food simulants. GB 5009.156 press operation.
3.2.2 1g/L aqueous sodium bicarbonate solution. Weigh 1g (accurate to 0.1g) of sodium bicarbonate, washed with water and dissolved in 1L volumetric flask.
3.2.3 sodium acetate buffer (pH = 3.6). Weigh 25.0g of sodium acetate trihydrate was dissolved in 350mL of water, was added 5.0mL phosphate, with about
50mL glacial acetic acid pH adjusted to 3.6, add water to 500mL.
3.2.4 50% acetic acid solution. Measure 50mL of glacial acetic acid in 100mL volumetric flask to volume with water.
3.3 Standard
3.3.1 terephthalic acid (C8H6O4, CAS Number. 100-21-0), purity ≥99%, or by the state certified and the certificate standard reference material
Reference material.
3.3.2 phthalic acid (C8H6O4, CAS Number. 88-99-3), purity ≥99%, or by the state certified and the certificate standard reference material
Reference material.
3.4 Standard Preparation
3.4.1 terephthalic acid standard stock solution (500mg/L). Weigh accurately 50mg (accurate to 0.1 mg) of terephthalic acid standard, plus
Into 90mL of methanol was dissolved, the solution was heated to 50 ℃, continued IH, terephthalic acid fully dissolved. After cooling the solution was transferred to a
100mL volumetric flask, diluted with methanol. Valid for six months.
3.4.2 terephthalic standard intermediate solution. 6 were added in 0mL 25mL volumetric flask, 1.0mL, 2.0mL, 5.0mL,
10.0mL, 20.0mL terephthalic acid standard stock solution, and then were added 5mL phthalate internal standard stock solution, diluted with methanol.
Acid intermediate solution concentration standards were 0.0mg/L, 20mg/L, 40mg/L, 100mg/L, 200mg/L, 400mg/L.
The concentration of the internal standard are phthalic acid 200mg/L. Day should be formulated.
3.4.3 water-based, acidic, alcoholic medium food simulant standard working solution. terephthalic acid were pipetted 2.0mL standard solution of intermediate
6 in 50mL volumetric flask, with the corresponding volume of food simulant. Water-based, acid, alcohol, food simulants standard terephthalate
Fluid concentrations of 0.0mg/L, 0.8mg/L, 1.6mg/L, 4.0mg/L, 8.0mg/L, 16.0mg/L; internal standard concentrations are
8.0mg/L.
3.4.4 Media olive oil standard working solution. Weigh 50g of olive oil in 6 250mL separatory funnel and accurately into 2.0mL
Intermediate terephthalic acid standard solution mixed uniformly 50mL of n-heptane was added, and then mixed. Sodium bicarbonate solution was added 20mL, fully
Oscillation 1min, 15min standing stratification. The lower aqueous phase was collected with 100mL beaker, then re-extracted with sodium bicarbonate solution was added 20mL
Upper oil phase. Standing after shaking, the two phases are separated, the lower layer was collected with a beaker of water and the combined aqueous phase was extracted twice with a solution. With a syringe or true
Vacuum pump (flow rate 10mL/min ~ 20mL/min) so that the extract via solid-phase extraction C18 column. The filtrate was collected in a 50mL volumetric flask, add
1.0mL50% acetic acid solution into water to volume. Take 1mL ~ 2mL filtrate was filtered through a membrane. Standard working solution concentration of terephthalic acid
Were 0.0mg/kg, 0.8mg/kg, 1.6mg/kg, 4.0mg/kg, 8.0mg/kg, 16.0mg/kg; internal standard concentrations are
8.0mg/kg.
3.4.5 phthalate internal standard stock solution (1000mg/L). 0.1 g of accurately weighed (accurate to 0.1 mg) phthalic acid standard, with
10mL of isopropanol was dissolved, then the solution was transferred to a 100mL volumetric flask and isopropanol to volume. Valid for six months.
3.4.6 phthalic acid intermediate solution of internal standard (200mg/L). Take 5mL phthalate internal standard stock solution was 25mL volumetric flask,
Diluted with methanol.
4 Equipment
4.1 HPLC. with UV detector and a 10μL loop.
4.2 Analytical balance. a sense of the amount of 0.1mg, 0.1g.
4.3 pH meter.
4.4 C18 solid phase extraction column. octadecylsilane (ODS) 400mg.
4.5 River microporous membrane. 0.45μm.
5 Step analysis
5.1 migration test sample
GB 5009.156 according to the requirements and GB 31604.1, the sample migration test, the test solution to give food simulants. If you get
The food simulant test solution can not be immediately next test, the test solution should be stored in food simulants dark at 4 ℃ refrigerator.
The resulting analog should be the next step after the test food was returned to room temperature or cooling the sample solution.
5.2 Preparation of test solution
5.2.1 Preparation of water-based, acid, alcohol, food simulant test solution
Pipette 50.0mL migration resulting from water-based assay in food simulants previously filled with 2.0mL phthalic intermediate internal standard solution
A 100mL Erlenmeyer flask, mixed, take 1mL ~ 2mL tested by membrane filtration.
5.2.2 Preparation of test solution olive oil mimetic
Weigh obtained from 50.0g olive oil migration the test medium food simulant in 250mL separatory funnel, internal standard was added 2.0mL
Intermediate solution, the amount of 50mL of n-heptane mixed in a separatory funnel. Then 3.4.4 "sodium bicarbonate solution was added 20mL
The filtrate was taken 1mL ~ 2mL membrane filtration "steps, the solution to be tested.
5.3 Preparation of the blank test solution
5.2 according to the process of step food simulant without contact with the food contact materials.
5.4 Determination
5.4.1 Liquid Chromatography reference condition
Referring liquid chromatography conditions are listed below.
a) Column. C18 column, column length 250mm, internal diameter 4.6mm, 5 m particle size, or equivalent person; b) Mobile phase. A. 150mL sodium acetate buffer (3.2.5) + 750mL water; B. methanol ;
Determination of water-based, acid, alcohol analog product sample solution. mobile phase A + B = 80 + 20 (volume ratio); olive oil mimetic assay
When the test solution. mobile phase A + B = 85 + 15 (volume ratio);
c) flow rate. 1.5mL/min;
d) Column temperature. room temperature;
e) Injection volume. 10μL; f) UV detector. wavelength of 242nm.
5.4.2 draw standard curve
Measured according to the conditions listed in 5.4.1, the standard working solution sequentially injected into HPLC. Standard working solution concentration of terephthalic acid
The abscissa, in units of "mg/L or mg/kg" said terephthalic acid/phthalic acid peak area ratio as the ordinate, are plotted standard
Quasi curve. Standard Solution chromatogram see Appendix A. FIG.
5.4.3 Determination of test solution
Sequentially sample solution and the blank test solution food simulants, blank value, to obtain terephthalic acid/phthalic acid peak area ratio.
6 expression analysis results
Obtained from the standard curve the concentration of the acid in a sample solution, according to GB 5009.156 calculated for migration, food contact material obtained
Migration of terephthalic acid materials and articles. The results rounded to two significant figures.
7 confirmed
When the above result exceeds a certain value migration limit (SML), liquid chromatography - tandem mass spectrometry confirmed or other effective means. Liquid chromatography
Spectral - Analysis of the chromatogram and reference conditions see Appendices B and C. tandem mass spectrometry
8. Precision
The absolute difference between two measurement results obtained under repeatable conditions not exceed 10% of the arithmetic mean.
9 Other
Water-based, acidic, alcoholic mimetic terephthalic acid detection limit of 0.3mg/L; olive oil mimetic terephthalic acid
The detection limit of 0.3mg/kg.
Water-based, acidic, alcoholic mimetic terephthalic acid quantification limit of 1.0mg/L; olive oil mimetic terephthalic acid
Quantitative limit of 1.0mg/kg.
Appendix A
Terephthalic standard chromatogram
Terephthalic standard chromatogram shown in Figure A. 1.
Figure A. One pair of standard chromatogram acid
Appendix B
Liquid chromatography - tandem mass spectrometry confirmed the reference condition
B. 1 HPLC conditions
HPLC conditions are listed below.
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