GB 31604.64-2025 National food safety standard - Food contact materials and products - Determination of migration of citrate and sebacate compounds English, Anglais, Englisch, Inglés, えいご
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National Standard of the People's Republic of China
GB 31604.64-2025
National Food Safety Standard - Food Contact Materials and Articles - Determination of migration of citrate and sebacate compounds
Issue date: 2025-09-02 Implementation date: 2026-03-02
Issued by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
the National Health Commission of the People’s Republic of China
Contents
Foreword
1 Scope
2 Principle
3 Reagents and Materials
4 Instruments and Equipment
5 Analytical Procedure
6 Expression of Analytical Results
7 Precision
8 Others
National Food Safety Standard
Food Contact Materials and Articles
Determination of migration of citrate and sebacate compounds
1 Scope
This standard specifies the determination of migration levels of triethyl citrate, di-n-butyl adipate, tri-n-butyl acetyl citrate, dibutyl sebacate, diisooctyl sebacate, and di(2,2,6,6-tetramethyl-4-piperidinyl) sebacate in food contact materials and articles.
This standard applies to the migration of triethyl citrate, di-n-butyl sebacate, tri-n-butyl acetyl citrate, Dioctyl sebacate, and Dioctyl sebacate di(2,2,6,6-tetramethyl-4-piperidyl) ester.
2 Principle
Migration testing of food contact materials and articles is conducted using food simulants or chemical substitute solvents. Water-based, acidic, and ethanol-containing food simulant immersion solutions are extracted with n-hexane before instrumental analysis. Extracts from lipid-containing food simulants are obtained via acetonitrile extraction. These extracts undergo matrix dispersion extraction purification and nitrogen blowdown concentration before instrumental analysis. Extracts from chemical substitute solvents (95% ethanol and iso-octane) are analyzed directly. Test solutions are separated via gas chromatography columns and detected by mass spectrometry, with quantification performed using the external standard method based on peak area.
3 Reagents and Materials
Unless otherwise specified, reagents used in this method are analytical grade. Water complies with Grade 1 water as defined by GB/T 6682. Avoid using plastic equipment that may contaminate analyses during testing. Glassware and equipment should be thoroughly cleaned before use.
3.1 Reagents
3.1.1 n-Hexane (C₆H₁₄): Chromatographic grade.
3.1.2 Acetonitrile (C₂H₃N): Chromatographic grade.
3.1.3 25% (w/w) ammonia solution.
3.1.4 Magnesium sulfate (MgSO₄).
3.1.5 Anhydrous ethanol (C₂H₆O): Chromatographic grade.
3.1.6 Glacial acetic acid (C₂H₄O₂).
3.1.7 Isooctane (C₈H₁₈): Chromatography grade.
3.1.8 Olive oil: Must comply with the specifications for lipid food simulants in GB 5009.156.
3.2 Materials
3.2.1 Ethylenediamine-N-propylsilane-modified silica gel (PSA): 40 μm to 60 μm.
3.2.2 Octadecylsilane-bonded silica gel (C18): 40 μm to 60 μm.
3.3 Reagent Preparation
3.3.1 Acidic, ethanol-containing, and lipid-containing food simulants and chemical substitute solvents: As specified in GB 31604.1 and GB 5009.156.
3.3.2 10% (w/w) Ammonia Solution: Measure 211 mL of 25% ammonia solution and 289 mL of water; mix thoroughly.
3.4 Reference Standards
3.4.1 Triethyl citrate (C₁₂H₂O₇, CAS No.: 77-93-0): Purity ≥98%, or a reference standard certified by a national authority and issued with a Certificate of Analysis.
3.4.2 Di-n-butyl sebacate (C₁₈H₃₄O₄, CAS No.: 109-43-3): Purity ≥98%, or a reference standard certified by a national authority and issued with a Certificate of Analysis.
3.4.3 Tri-n-butyl acetyl citrate (C₂₀H₃₄O₈, CAS No.: 77-90-7): Purity ≥98%, or a standard material certified and granted a certificate of analysis by a national authority.
3.4.4 Di(2-ethylhexyl) sebacate (C₂₆H₅₀O₄, CAS No.: 122-62-3): Purity ≥98%, or a standard material certified and granted a certificate of analysis by a national authority.
3.4.5 Diisooctyl sebacate (C₂₆H₅₀O₄, CAS No.: 27214-90-0): Purity ≥98%, or a reference standard certified by a national authority and granted a Certificate of Analysis.
3.4.6 Di(2,2,6,6-tetramethyl-4-piperidinyl) sebacate (C₂₈H₅₂N₂O₄, CAS No.: 52829-07-9): Purity ≥98%, or a reference standard certified by a national authority and granted a Certificate of Analysis.
3.5 Preparation of Standard Solutions
3.5.1 Preparation of Single Standard Stock Solution (1000 mg/L)
Accurately weigh 10 mg (to 0.1 mg precision) each of triethyl citrate, di-n-butyl sebacate, tri-n-butyl acetyl citrate, dihydroxydecanedioic acid di(2-ethylhexyl) ester, diisooctyl sebacate, and di(2,2,6, 6-Tetramethyl-4-Piperidyl) Adipate. Dissolve each in n-hexane, transfer to a 10 mL brown volumetric flask, dilute to the mark with n-hexane, and mix thoroughly. Transfer the solution to a brown glass bottle. Store protected from light at 0°C to 4°C in a refrigerator. Shelf life: 6 months.
3.5.2 Preparation of Mixed Standard Intermediate Solution A (100 mg/L)
Accurately pipette 1.00 mL of each of the above 6 single standard stock solutions into the same 10 mL brown volumetric flask. Accurately dilute to the mark with anhydrous ethanol, mix thoroughly, and transfer the solution to a brown glass bottle. Store in a refrigerator at 0°C to 4°C protected from light. Shelf life: 3 months.
3.5.3 Preparation of Mixed Standard Intermediate Solution B (100 mg/L)
Accurately pipette 1.00 mL of each of the above 6 single standard stock solutions into the same 10 mL brown volumetric flask. Accurately dilute to the mark with n-hexane, mix thoroughly, and transfer the solution to a brown glass bottle. Store in a refrigerator at 0°C to 4°C protected from light. Shelf life: 3 months.
3.5.4 Standard Working Solution of Acidic Food Simulants
Pipette 5.00 mL of 4% acetic acid into 6 graduated glass tubes. Accurately transfer 0 mL, 0.020 mL, 0.10 mL, 0.20 mL, 0.40 mL, and 0.50 mL of mixed standard intermediate solution A into each tube. Add 4% acetic acid and dilute to 10 mL. After mixing, accurately transfer 2.4 mL of 10% (w/w) ammonia solution. Then add 5.00 mL of n-hexane to each, vortex for 5 min, centrifuge at 4000 r/min for 5 min, transfer the upper hexane layer to a clean volumetric flask, repeat the procedure with 5.00 mL hexane, combine both solutions, and dilute to 10 mL with hexane. This yields mixed standard working solutions with concentrations of 0 mg/L, 0.20 mg/L, 1.0 mg/L, 2.0 mg/L, 4.0 mg/L, and 5.0 mg/L. Prepare fresh solutions as needed.
3.5.5 Water and Ethanol-Containing Food Simulants Standard Working Solutions
Pipette 5.00 mL of food simulant into 6 graduated glass tubes. Using a pipette, accurately transfer 0 mL, 0.020 mL, 0. 10 mL, 0.20 mL, 0.40 mL, and 0.50 mL of mixed standard intermediate solution A. Add the corresponding food simulant and dilute to 10 mL. After mixing, accurately pipette 0.25 mL of 10% (w/w) ammonia solution, then add 5.00 mL of hexane. vortex-agitate for 5 min, centrifuge at 4,000 rpm for 5 min, transfer the upper hexane layer to a clean volumetric flask, repeat the procedure with 5.00 mL hexane, combine both solutions, and dilute to 10 mL with hexane. Obtain mixed standard working solutions with concentrations of 0 mg/L, 0.20 mg/L, 1.0 mg/L, 2.0 mg/L, 4.0 mg/L, and 5.0 mg/L. Prepare fresh solutions for immediate use.
3.5.6 Standard Working Solution for Fat-Containing Food Simulants
