GB 31604.43-2016National food safety standard - Food contact materials and products - Determination of migration quantity of ethylenediamine and hexamethylene diamine (English PDF)

3.1 Reagents

3.1.1 Ethyl chloroformate (C3H5ClO2). Purity is greater than 97%.

3.1.2 Glacial acetic acid (C2H4O2).

3.1.3 Anhydrous ethanol (C2H6O).

3.1.4 Toluene (C7H8).

3.4 Standard solution preparation

3.4.1 Ethylenediamine stock solution prepared by water (1000mg/L).

Accurately WEIGH 50mg (accurate to 0.1mg) of ethylenediamine; PLACE it

into 50mL volumetric flask; USE water to dilute it.

3.4.2 Hexamethylene diamine stock solution prepared by water (500mg/L).

Accurately WEIGH 25mg (accurate to 0.1mg) of hexamethylene diamine;

PLACE it into 50mL volumetric flask; USE water to dilute it.

3.4.3 Propane diamine stock solution prepared by water (500mg/L). Accurately

WEIGH 25mg (accurate to 0.1mg) of propane diamine; PLACE it into 50mL

volumetric flask; USE water to dilute it.

3.4.4 Ethylenediamine stock solution prepared by toluene (1000mg/L).

Accurately WEIGH 50mg (accurate to 0.1mg) of ethylenediamine; PLACE it

into 50mL volumetric flask; USE toluene to dilute it.

3.4.5 Hexamethylene diamine stock solution prepared by toluene (500mg/L).

Accurately WEIGH 25mg (accurate to 0.1mg) of hexamethylene diamine;

PLACE it into 50mL volumetric flask; USE toluene to dilute it.

3.4.6 Propane diamine stock solution prepared by toluene (500mg/L).

Accurately WEIGH 25mg (accurate to 0.1mg) of propane diamine; PLACE it

into 50mL volumetric flask; USE toluene to dilute it.

The prepared stock solution can be stored in dark place at 5°C~20°C, and it is

valid within 3 months.

3.5 Vessels and materials

3.5.1 Glass bottle. 2mL, 10mL, the caps are coated with Teflon-coated butyl

rubber or silicone rubber gaskets.

3.5.2 Volumetric flask. 50mL.

3.5.3 Micro-syringes. 10µL and 25µL.

3.5.4 Oscillator.

4.1 Gas chromatograph. equipped with hydrogen flame ionization detector and

data automatic analysis software.

4.2 Analytical balance. Sensitivity is 0.0001g and 0.01g.

When food contact materials and products are contacted with olive oil at 10d,

20°C or 10d, 40°C for a long period of time, ethylenediamine and

hexamethylene diamine that have migrated from food contact materials and

products react with olive oil, which results in lower test results. Ethanol solution

(95%, volume fraction) or isooctane shall be used to replace oil-based food

simulants for testing.

5.1.2.2 Water-based, acidic food, alcoholic food simulants

Accurately MEASURE 1mL of the water-based, acidic food, and alcoholic food

simulants obtained from the migration test; PLACE it into 10mL glass bottle;

ADD 10µL of propane diamine stock solution prepared by water; COVER and

SEAL it; MIX it uniformly.

5.1.2.3 Oil-based food simulant

Accurately WEIGH 1.0g (accurate to 0.01g) of the oil-based food simulant

obtained from the migration test; PLACE it into 10mL sample bottle; ADD 10µL

of propane diamine stock solution prepared by toluene; COVER and SEAL it;

MIX it uniformly.

5.1.2.4 Ethanol solution (95%, volume fraction)

Accurately MEASURE 1.0mL of the ethanol solution (95%, volume fraction)

obtained from the migration test; PLACE it into 10mL sample bottle; ADD 10µL

of propane diamine stock solution prepared by water; COVER and SEAL it;

MIX it uniformly.

5.1.2.5 Isooctane

Accurately MEASURE 1.0mL of the isooctane obtained from the migration test;

PLACE it into 10mL sample bottle; ADD 10µL of propane diamine stock

solution prepared by toluene; COVER and SEAL it; MIX it uniformly.

5.1.3 Preparation of blank test solution

Handle the food simulants that have not been in contact with food contact

materials and products in accordance with the operation of 5.1.2.

5.2 Derivatization of food simulant test solution

5.2.1 Water-based, acidic food, alcoholic food simulant and ethanol

solution (95%, volume fraction)

ADD 1mL of ammonia solution (3%, volume fraction), 3mL of sodium

hydroxide solution (5mol/L), 2mL of toluene, and 200µL of ethyl chloroformate

into the glass bottle which contains water-based, acidic food, and alcoholic

c) Detector temperature. 300°C;

d) Furnace temperature. keep for 1min at 100°C, rise to 270 at 25°C/min,

keep for 7min;

e) Carrier gas. nitrogen, flow rate 1.8mL/min;

f) Sample injection mode. split injection, split ratio 10.1;

g) Injection volume. 1µL.

5.4.2 Drawing of standard curve

Conduct derivatization for the standard working solution prepared in 5.1.1

according to 5.2; TEST it under the instrument parameters listed in 5.4.1. With

the concentration of ethylenediamine or hexamethylene diamine in the

standard working solution of food simulants as abscissa, AND the ratio of the

peak area between the corresponding ethylenediamine derivative or

hexamethylene diamine derivative and internal standard substance propane

diamine derivative as vertical axis, DRAW a standard working curve; OBTAIN

a linear equation. See Appendix A for the chromatograms of standard solution.

5.4.3 Quantitative determination

After the sequential sample injection of derivatized food simulant test solution

and blank test solution, OBTAIN the corresponding ratio of the peak area of

ethylenediamine derivative or hexamethylene diamine derivative and internal

standard substance propane diamine derivative, respectively; OBTAIN the

content of ethylenediamine or hexamethylene diamine in the sample solution

according to the standard curve; DEDUCT blank value.