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Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 31604.64-2025: National food safety standard - Food contact materials and products - Determination of migration of citrate and sebacate compounds Status: Valid
Basic dataStandard ID: GB 31604.64-2025 (GB31604.64-2025)Description (Translated English): National food safety standard - Food contact materials and products - Determination of migration of citrate and sebacate compounds Sector / Industry: National Standard Classification of Chinese Standard: C53 Word Count Estimation: 12,199 Date of Issue: 2025-09-02 Issuing agency(ies): National Health Commission; State Administration for Market Regulation GB 31604.64-2025: National food safety standard - Food contact materials and products - Determination of migration of citrate and sebacate compounds---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GB31604.64-2025 National Standards of the People's Republic of China National Food Safety Standards Citrates and food contact materials and articles Determination of migration of sebacic acid esters Published on 2025-09-02 Implemented on 2026-03-02 National Health Commission of the People's Republic of China State Administration for Market Regulation issued National Food Safety Standards Citrates and food contact materials and articles Determination of migration of sebacic acid esters 1.Scope This standard specifies the requirements for triethyl citrate, di-n-butyl sebacate, acetylated tributyl citrate, and sebacate in food contact materials and articles. Methods for determining the migration of di(2-ethylhexyl) ester, diisooctyl sebacate, and di(2,2,6,6-tetramethyl-4-piperidine) sebacate. This standard applies to triethyl citrate and sebacic acid in food contact materials and products such as plastics, rubber, adhesives, coatings and paints, and paper. Di-n-butyl ester, tributyl acetylacetonate, di(2-ethylhexyl) sebacate, diisooctyl sebacate, and di(2,2,6,6-tetramethyl- Determination of the migration of 4-piperidine esters. 2.Principle Migration tests are conducted on food contact materials and articles using food simulants or chemical substitute solvents, including aqueous, acidic, and ethanol-containing food simulants. The extract of the food simulant was extracted with hexane and then analyzed; the extract of the food simulant containing oil was extracted with acetonitrile, and the extract was then subjected to matrix dispersion extraction. The solution was concentrated by chemical or nitrogen blowing before being analyzed by gas chromatography; the solution with chemically substituted solvents (95% ethanol and isooctane) was directly analyzed by gas chromatography. Column separation, mass spectrometry detection, and external standard method for peak area quantification. 3.Reagents and Materials Unless otherwise specified, all reagents used in this method are of analytical grade, and the water is Grade I water as specified in GB/T 6682.Avoidance of certain precautions during the experiment is recommended. Use any plastic equipment that may contaminate the analysis. 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% (mass fraction) 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). chromatographic grade. 3.1.8 Olive oil. It shall comply with the provisions of GB 5009.156 on simulants of oils and fats. 3.2 Materials 3.2.1 Ethylenediamine-N-propylsilane-modified silica gel filler (PSA). 40μm~60μm. 3.2.2 Octadecylsilane bonded silica filler (C18). 40μm~60μm. 3.3 Reagent Preparation 3.3.1 Acidic, ethanol-containing and oil-containing food simulants and chemical alternative solvents. in accordance with the provisions of GB 31604.1 and GB 5009.156. 3.3.2 10% (mass fraction) ammonia solution. Measure 211 mL of 25% ammonia solution and 289 mL of water, and mix well. 3.4 Standard Products 3.4.1 Triethyl citrate (C12H2O7, CAS No.. 77-93-0). Purity ≥ 98%, or certified by the state and granted a standard substance certificate. Standard product. 3.4.2 Di-n-butyl sebacate (C18H34O4, CAS No.. 109-43-3). Purity ≥98%, or certified by the state and granted a standard substance certificate. Standard edition of the book. 3.4.3 Acetyl tributyl citrate (C20H34O8, CAS No.. 77-90-7). Purity ≥98%, or certified by the state and granted a standard substance certificate. Standard edition of the book. 3.4.4 Di(2-ethylhexyl) sebacate (C26H50O4, CAS No.. 122-62-3). Purity ≥98%, or certified by the state and granted a standard. Standard materials for material certificates. 3.4.5 Diisooctyl sebacate (C26H50O4, CAS No.. 27214-90-0). Purity ≥98%, or certified by the state and granted as a standard substance. Standard products for certificates. 3.4.6 Di(2,2,6,6-tetramethyl-4-piperidine) sebacate (C28H52N2O4, CAS No.. 52829-07-9). Purity ≥98%, or certified by national standards. Standards that are certified and granted a certificate of reference material by the state. 3.5 Preparation of Standard Solutions 3.5.1 Preparation of a single standard stock solution (1000 mg/L) Accurately weigh 10 mg (accurate to 0.1 mg) of triethyl citrate, di-n-butyl sebacate, acetylated tributyl citrate, and sebacate, respectively. Standards of di(2-ethylhexyl) ester, diisooctyl sebacate, and di(2,2,6,6-tetramethyl-4-piperidine) sebacate were dissolved in n-hexane and then transferred... Transfer to a 10 mL brown volumetric flask, dilute to the mark with n-hexane and mix well. Transfer the solution to a brown glass bottle and incubate at 0°C–4°C. Store in a light-proof box. Shelf life is 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 six single standard stock solutions into the same 10 mL brown volumetric flask, and dilute with anhydrous ethanol. After confirming the volume is reached, shake well and transfer the solution to a brown glass bottle. Store in a refrigerator at 0℃~4℃, away from light. Shelf life is 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 six single standard stock solutions into the same 10 mL brown volumetric flask, and accurately dilute with n-hexane. After bringing the volume to the mark, shake well and transfer the solution to a brown glass bottle. Store in a refrigerator at 0℃~4℃, protected from light. Shelf life is 3 months. 3.5.4 Standard working solution of acidic food simulants Pipette 5.00 mL of 4% acetic acid into six graduated glass tubes, and accurately transfer 0 mL, 0.020 mL, 0.10 mL, 0.20 mL, and 0.5 mL into each tube. Mix 0.40 mL and 0.50 mL of standard intermediate solution A, add 4% acetic acid and bring the volume to 10 mL. After mixing well, accurately transfer 2.4 mL of 10% acetic acid solution. Add (mass fraction) ammonia water, then add 5.00 mL of n-hexane, vortex extract for 5 min, centrifuge at 4000 r/min for 5 min, and take... Transfer the upper layer of n-hexane solution to a clean volumetric flask, then add 5.00 mL of n-hexane to each flask and repeat the above steps. Combine the two solutions and use them together. The solution was diluted to 10 mL with n-hexane. This yielded solutions with mass concentrations of 0 mg/L, 0.20 mg/L, 1.0 mg/L, 2.0 mg/L, 4.0 mg/L, and [other concentrations not specified]. A 5.0 mg/L mixed standard working solution. Prepare fresh before use. 3.5.5 Water and Ethanol-containing Food Simulator Standard Working Solutions Pipette 5.00 mL of food simulant into each of six graduated glass tubes. Accurately pipette 0 mL, 0.020 mL, and... Mix 0.10 mL, 0.20 mL, 0.40 mL, and 0.50 mL of standard intermediate solution A, add the corresponding food simulant, and bring the volume to a final depth. After mixing 10 mL of the solution, accurately transfer 0.25 mL of 10% (mass fraction) ammonia solution, add 5.00 mL of n-hexane, and vortex to extract. Centrifuge at 4000 rpm for 5 min, transfer the supernatant hexane solution to a clean volumetric flask, and add 5.00 mL of hexane to each flask. Repeat the above steps, combine the two solutions, and bring the volume to 10 mL with n-hexane. This yields solutions with mass concentrations of 0 mg/L, 0.20 mg/L, and... Mixed standard working solutions of 1.0 mg/L, 2.0 mg/L, 4.0 mg/L and 5.0 mg/L. Prepare fresh before use. 3.5.6 Standard working solutions for simulants of oily foods Weigh 3.0g (accurate to 0.1g) of olive oil into six glass test tubes, and accurately transfer 0mL, 0.015mL, 0.030mL, and 0.015mL into each tube. Mix 0.060 mL, 0.12 mL, and 0.15 mL of a mixed standard intermediate solution B, then add 0.25 mL of 10% (mass fraction) ammonia solution. 3.00 mL acetonitrile, vortex for 5 min, allow to stand for separation, and transfer the upper acetonitrile solution to a clean volumetric flask. Add 3.00 mL acetonitrile... The nitrile extraction was repeated once, and the two extracts were combined and centrifuged in a 15 mL container containing 900 mg magnesium sulfate, 150 mg PSA, and 150 mg C18. Centrifuge at 4000 rpm for 5 min in the tube. Take 4.00 mL of the upper acetonitrile solution, blow it to near dryness with nitrogen, and then make up to 1.00 mL with acetonitrile to obtain... Mixed standards with mass concentrations of 0 mg/kg, 0.50 mg/kg, 1.0 mg/kg, 2.0 mg/kg, 4.0 mg/kg and 5.0 mg/kg were prepared. Working solution. Prepare fresh before use. 3.5.7 Standard working solutions with chemically alternative solvents (95% ethanol and isooctane) 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 B into six separate containers. In a 10 mL volumetric flask, dilute to the mark with 95% ethanol or isooctane and shake well to obtain concentrations of 0 mg/L, 0.20 mg/L, and [other concentrations not specified]. Mixed standard working solutions of 1.0 mg/L, 2.0 mg/L, 4.0 mg/L and 5.0 mg/L. Prepare fresh before use. 4.Instruments and Equipment 4.1 Gas Chromatography-Mass Spectrometry (GC-MS). equipped with an electron impact ion source. 4.2 Electronic balance. sensitivity is 0.0001g and 0.1g respectively. 4.3 Vortex Oscillator. 4.4 Pipettes. with capacities of.200 μL, 1.00 mL and 10.00 mL. 4.5 Centrifuge. Maximum speed ≥ 4000 r/min. 4.6 Nitrogen blowing device. 5.Analysis Steps 5.1 Preparation of test solution 5.1.1 Migration Test Food contact materials and articles shall undergo migration testing in accordance with the provisions of GB 31604.1 and GB 5009.156.The immersion solution obtained from the migration test shall be... If immediate testing is not possible, store in a refrigerator at 0°C–4°C, protected from light, and for no more than 72 hours. If further testing is to be conducted, [the following steps should be taken]. Use the soaking solution only after it has returned to room temperature. 5.1.2 Treatment of Acidic Food Simulator Immersion Solution Accurately transfer 10.00 mL of the soaking solution into a glass test tube, mix well, then accurately transfer 2.4 mL of 10% (mass fraction) ammonia solution, and add... 5.00 mL of n-hexane was added, and the mixture was extracted by vortexing for 5 min. After centrifugation at 4000 rpm for 5 min, the supernatant n-hexane solution was transferred to a clean volumetric flask. Add 5.00 mL of n-hexane and repeat the above steps. Combine the two solutions and dilute to 10 mL with n-hexane. Take the supernatant for instrument analysis. 5.1.3 Treatment of water and ethanol-containing food simulant soaking solutions Accurately transfer 10.00 mL of the soaking solution into a glass test tube, mix well, then accurately transfer 0.25 mL of 10% (mass fraction) ammonia solution, and add... 5.00 mL of n-hexane was added, and the mixture was extracted by vortexing for 5 min. After centrifugation at 4000 rpm for 5 min, the supernatant n-hexane solution was transferred to a clean volumetric flask. Add 5.00 mL of n-hexane and repeat the above steps. Combine the two solutions and dilute to 10 mL with n-hexane. Take the supernatant for instrument analysis. 5.1.4 Treatment of immersion solutions containing fat-containing food simulants Accurately weigh 3.0 g (accurate to 0.01 g) of olive oil infusion into a glass test tube, add 0.25 mL of 10% (mass fraction) ammonia solution and... 3.00 mL acetonitrile, vortex for 5 min, allow to stand for separation, and transfer the supernatant to a clean volumetric flask. Repeat the extraction once more, and combine the two extracts. The extract was transferred to a 15 mL centrifuge tube containing 900 mg magnesium sulfate, 150 mg PSA, and 150 mg C18, and centrifuged at 4000 rpm. 5 min. Take 4.00 mL of the upper acetonitrile solution, blow it with nitrogen until nearly dry, then make up to 1.00 mL with acetonitrile, and take the clear liquid for instrument analysis. 5.1.5 Treatment of Immersion Solutions with Chemical Alternative Solvents (95% Ethanol and Isooctane) The clear liquid obtained after the migration test is used for instrument analysis. 5.1.6 Blank Test Food simulants and chemical substitute solvents that have not come into contact with food contact materials and products were treated according to sections 5.1.2 to 5.1.5 respectively to obtain blank samples. The test solution is ready for instrumental analysis. 5.2 Instrument Reference Conditions a) Chromatographic column. 50% phenyl-methylpolysiloxane quartz capillary column, 30m long, 0.25mm inner diameter, 0.25μm film thickness, or Equivalent column; b) Temperature program. Initial temperature 150℃, hold for 0 min, increase to 320℃ at a rate of 10℃/min, hold for 3 min; c) Inlet temperature. 280℃; d) Ion source temperature. 280℃; e) Transmission line temperature. 330℃; f) Carrier gas. Helium (purity ≥ 99.999%), constant flow mode, flow rate 1.5 mL/min; g) Injection method. split injection, split ratio 5.1; h) Injection volume. 1 μL; i) Ionization method. EI; j) Solvent delay. 3.0 min; k) Mass spectrometry scanning mode. Selected ion mode (SIM); l) For the qualitative and quantitative ions of each target analyte, please refer to Appendix A. 5.3 Preparation of Standard Working Solutions The standard working solution was measured according to the instrument reference conditions listed in 5.2.The determinations were performed using triethyl citrate and decanoate in the standard working solution, respectively. Dibutyl diacidate, Tributyl acetylacetonate, Di(2-ethylhexyl) sebacate, Diisooctyl sebacate, Di(2,2,6,6-tetramethyl) sebacate A standard working curve was plotted with the mass concentration of methyl-4-piperidine ester on the x-axis and the corresponding quantitative ion peak area on the y-axis. (6 types of...) See Appendix B for the total ion chromatogram of the standard working solution of the analyte. 5.4 Determination of Sample Solution 5.4.1 Qualitative Judgment According to the instrument conditions listed in 5.2, the sample solution and the standard working solution were measured separately. If the sample solution and the standard working solution have similar properties... The corresponding chromatographic peak retention time deviation is within ±0.5%, and in the mass spectrum of the sample solution after background subtraction, the selected peak retention time deviation is within ±0.5%. All ions appear, and the signal-to-noise ratio is not less than 3.The relative abundance ratio of qualitative ions in the mass spectrum of the sample solution is compared with that of a standard working solution with a concentration close to that of the standard working solution. ...... Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 31604.64-2025_English be delivered?Answer: Upon your order, we will start to translate GB 31604.64-2025_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of GB 31604.64-2025_English with my colleagues?Answer: Yes. The purchased PDF of GB 31604.64-2025_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.Question 3: Does the price include tax/VAT?Answer: Yes. 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