National food safety standard - Food contact materials and articles - Determination of migration of 5-Ethylidene-2-norbornene, mixt. of endo-and exo-isomers
National Standard of the People’s Republic of China
GB 31604.53-2022
National food safety standard
Food contact materials and articles
Determination of migration amount of 5-ethylidene-2-norbornene
食品安全國家標準
食品接觸材料及制品
5-亞乙基-2-降冰片烯遷移量的測定
(English Translation)
Issue date: 2022-06-30 Implementation date: 2022-12-30
Issued by the National Health Commission of the People's Republic of China
the State Administration for Market Regulation of the People's Republic of China
Contents
1 Scope 1
2 Principle 1
3 Reagents and materials 1
4 Apparatus 3
5 Analytical procedures 3
6 Expression of analysis results 7
7 Precision 8
8 Others 8
Annex A Reference spectrums for 5-ethylidene-2-norbornene 9
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
National food safety standard
Food contact materials and articles
Determination of migration amount of 5-ethylidene-2-norbornene
1 Scope
This standard specifies the determination method for migration amount of 5-ethylidene-2-norbornene in food contact materials and articles.
This standard is applicable to the determination of migration amount of 5-ethylidene-2-norbornene in plastic-, rubber-, and coating-type food contact materials and articles.
2 Principle
After the migration test on food contact materials and articles in accordance with the provisions of GB 31604.1 and GB 5009.156, 5-ethylidene-2-norbornene in food simulants, i.e., 4% (v/v) acetic acid, 10% (v/v) ethanol, 20% (v/v) ethanol, 50% (v/v) ethanol and olive oil, by headspace injection, and that in chemical substitute solvents, i.e., 95% (v/v) ethanol and isooctane, by liquid injection, is determined using gas chromatography-mass spectrometry, with quantification performed by the external standard method based on the peak area.
3 Reagents and materials
Unless otherwise specified, analytically pure reagents, and Class-I water as defined in GB/T 6682, are used for the purpose of this method.
3.1 Reagents
3.1.1 Glacial acetic acid (C2H4O2).
3.1.2 Anhydrous ethanol (C2H6O).
3.1.3 Isooctane (C8H18).
3.1.4 Olive oil: Must comply with the requirements of GB 5009.156, Annex A.
3.1.5 N-hexane (C6H14): Chromatographically pure.
3.1.6 Tetrahydrofuran (C4H8O): Chromatographically pure.
3.2 Reagent preparation
Acidic and ethanol-containing food simulants: Prepared in accordance with GB 5009.156.
3.3 Standard substance
5-ethylidene-2-norbornene (C9H12, CAS No.: 16219-75-3): With a purity of ≥98%, or a standard substance certified by the state and granted a standard substance certificate.
3.4 Preparation of standard solutions
3.4.1 5-ethylidene-2-norbornene standard stock solution (1,000mg/L)
Accurately weigh 25mg (to the nearest of 0.1mg) of 5-ethylidene-2-norbornene standard substance, dissolve it in n-hexane, transfer the resultant solution to a 25-mL brown volumetric flask, dilute it to the scale with n-hexane, and mix well. Then, transfer the solution to a brown glass container and store it at 0℃~4℃ away from light, with a shelf life of 3 months.
3.4.2 5-ethylidene-2-norbornene intermediate standard solution (100mg/L)
Pipette 2.50mL of the 5-ethylidene-2-norbornene standard stock solution (1,000mg/L) into a 25-mL brown volumetric flask, dilute it to the scale with n-hexane, and mix well. Then, transfer the solution to a brown glass container and store it at 0℃~4℃ away from light, with a shelf life of 3 months.
3.4.3 5-ethylidene-2-norbornene intermediate standard solution A
Pipette 0.15mL, 0.30mL, 0.50mL, 1.50mL, and 3.00mL of the 5-ethylidene-2-norbornene intermediate standard solution (100mg/L) into separate 5-mL volumetric flasks, dilute the solutions to the scale with tetrahydrofuran, and mix well. The concentrations of the series of intermediate standard solutions thus prepared are equivalent to 3.0mg/L, 6.0mg/L, 10mg/L, 30mg/L, and 60mg/L, respectively. Then, transfer the solutions to separate brown glass containers and store them at 0℃~4℃ away from light, with a shelf life of 1 month.
3.4.4 5-ethylidene-2-norbornene intermediate standard solution B
Pipette 0.15mL, 0.30mL, 0.50mL, 1.50mL, and 3.00mL of the 5-ethylidene-2-norbornene intermediate standard solution (100mg/L) into separate 5-mL volumetric flasks, dilute the solutions to the scale with n-hexane, and mix well. The concentrations of the series of intermediate standard solutions thus prepared are equivalent to 3.0mg/L, 6.0mg/L, 10mg/L, 30mg/L, and 60mg/L, respectively. Then, transfer the solutions to separate brown glass containers and store them at 0℃~4℃ away from light, with a shelf life of 1 month.
3.4.5 Standard working solutions of acidic and ethanol-containing food simulants
Add 5mL of food simulant without 5-ethylidene-2-norbornene into each of five headspace vials, then sequentially add 0.050mL of 5-ethylidene-2-norbornene intermediate standard solution A to each vial, immediately cap and seal the vials, and shake well. The concentrations of the standard working solutions thus prepared are 0.030mg/L, 0.060mg/L, 0.10mg/L, 0.30mg/L, and 0.60mg/L, respectively. Prepare a series of standard working solutions of acidic and ethanol-containing food simulants in this manner. Prepare them immediately before use.
3.4.6 Standard working solutions of oily food simulants
Add 5g of olive oil without 5-ethylidene-2-norbornene into each of five headspace vials, then sequentially add 0.050mL of 5-ethylidene-2-norbornene intermediate standard solution B to each vial, immediately cap and seal the vials, and shake well. The concentrations of the standard working solutions thus prepared are 0.030mg/kg, 0.060mg/kg, 0.10mg/kg, 0.30mg/kg, and 0.60mg/kg, respectively. Prepare them immediately before use.
3.4.7 Standard working solutions of chemical substitute solvents
Pipette 0.050mL of 5-ethylidene-2-norbornene intermediate standard solution B into each of five 5-mL volumetric flasks, add chemical substitute solvent to the scale, and mix well. The concentrations of the standard working solutions thus prepared are 0.030mg/L, 0.060mg/L, 0.10mg/L, 0.30mg/L, and 0.60mg/L, respectively. Prepare a series of standard working solutions of 95% (v/v) ethanol and isooctane in this manner. Prepare them immediately before use.
1 Scope
2 Principle
3 Reagents and materials
4 Apparatus
5 Analytical procedures
6 Expression of analysis results
7 Precision
8 Others
Annex A Reference spectrums for 5-ethylidene-2-norbornene
