GB 31604.11-2016National food safety standard - Food Contact Materials and Articles - Determination of Migration of 1,3-benzenedimethanamine (English PDF)

3.1 Reagents

3.1.1 Water-based, acidic, alcohol-based, oil-based food simulants. reagents

used in accordance with the provisions of GB 31604.1

3.1.2 Methanol (CH4O, CAS No.. 67-56-1). chromatographic pure

3.1.3 Tetrahydrofuran (C4H8O, CAS No. 109-99-9). chromatographic pure

3.1.4 Acetone (C3H6O, CAS No. 67-64-1)

3.1.5 Heptane (C7H16, CAS No.. 142-82-5)

3.1.6 Acetic acid (C2H4O2, CAS No.. 64-19-7)

Weigh 50 mg (nearest to 0.0001 g) of 1,3-benzenedimethylamine. Dissolve with

water. Set volume to 50 mL. The concentration shall be 1000 mg/L. This

solution shall be stored in the darkness at 5°C for three months.

3.4.2 1,3-benzenedimethylamine standard working solution used for

water-based (acidic, alcoholic) food simulants

Pipette 0.20 mL of 1,3-benzenedimethanamine standard stock solution (3.4.1)

in a 100mL volumetric flask with a graduated pipette. Dilute to scale with a

water-based (acidic, alcoholic) food simulant to obtain a 1,3-

benzenedimethanamine standard working solution for water-based (acidic,

alcoholic) food simulants with a concentration of 2.0 mg/L. This solution shall

be stored in the darkness at 5°C for one month.

3.4.3 1,3-benzenedimethylamine standard working solution used for oil-

based simulants

Pipette 2.0 mL of 1,3-xylylenediamine standard stock solution (3.4.1) in a 100

mL volumetric flask with a graduated pipette. Dilute to scale with water to obtain

a solution with a concentration of 20.0 mg/L. Pipette 10 mL of this solution in a

5.1 Sample migration test

In accordance with the requirements of GB 5009.156 and GB 31604.1, carry

out the sample migration test so as to obtain food simulant test solution. If the

resulting food simulant test solution cannot be immediately used for the next

test, the food simulant test solution shall be stored in a 4°C refrigerator from

light.

The resulting food simulant test solution shall be cooled or returned to room

temperature before proceeding to the next test.

5.2 Preparation of test solution

5.2.1 Preparations of water-based and alcohol food simulants

Pipette 2.0 mL of a water-based (alcoholic) food simulant obtained from the

migration test in a 5-mL tube with a graduated pipette. Add 0.4 mL of borate

buffer, mixing well. Then add 300 µL of fluorescent amine solution derivatization

reagent, oscillating 1min, placing still 10min. The derivative solution is filtered

through a 0.45 µm filter for high performance liquid chromatography injection.

5.2.2 Preparation of acidic food simulants

Pipette 10.0 mL of acidic food simulants from the migration test in a 25-mL

beaker by using a graduated pipette. Drop 5 mol/L sodium hydroxide solution

(3.2.4) with same volume as sodium hydroxide solution in 3.4.5, well mixing

(solution pH shall be within 8.0~9.9). Pipette 2.0 mL of the above solution in a

5-mL tube with a graduated pipette. The rest shall follow "add 0.4 mL of borate

buffer.for high performance liquid chromatography injection" in 5.2.1.

5.2.3 Preparation of oil-based food simulants

Weigh 20.0g (nearest to 0.01 g) olive oil mimics placing in a 125-mL separating

funnel. Separately add 1 mL of tetrahydrofuran solution and 5.0 mL of heptane.

After thoroughly mixing, add 20 mL of acetic acid solution, oscillating 5min,

placing still 15min. After the two phases are completely separated, collect the

aqueous phase. Pipette 10.0 mL of the above solution in a 25-mL beaker by

using a graduated pipette. Drop 5 mol/L sodium hydroxide solution (3.2.4) with

same volume as sodium hydroxide solution in 3.4.6, well mixing (solution pH

shall be within 8.0~9.9). Pipette 2.0 mL of the above solution in a 5-mL tube

with a graduated pipette. The rest shall follow "add 0.4 mL of borate buffer.for

high performance liquid chromatography injection" in 5.2.1.

5.3 Preparation of blank solution

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