GB 31604.10-2016 English PDF (GB31604.10-2016)
GB 31604.10-2016 English PDF (GB31604.10-2016)
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GB 31604.10-2016: National Food Safety Standard -- Food Contact Materials and Articles -- Determination of migration of 2,2-bis (4-hydroxyphenyl) propane (bisphenol A)
GB 31604.10-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Food contact materials and products -
Determination of migration quantity of 2,2-bis(4-
hydroxyphenyl) propane (bisphenol A)
食品接触材料及制品
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. MARCH 1, 2017
Issued by. National Health and Family Planning Commission of the PRC
Table of Contents
1 Scope .. 3
2 Principles .. 3
3 Reagents and materials . 3
4 Analytical procedures . 4
5 Analysis results expression . 7
6 Precision . 8
7 Others . 8
Appendix A Reference Mass Spectrometry Conditions . 9
National food safety standard -
Food contact materials and products -
Determination of migration quantity of 2,2-bis(4-
hydroxyphenyl) propane (bisphenol A)
1 Scope
This standard specifies the method for determining bisphenol A migration
quantity in food contact materials and products (PVC, polycarbonate, epoxy
resin and molded products).
This standard applies to liquid chromatography-mass spectrometry/mass
spectrometry detection of bisphenol A migration quantity in food contact
materials and products (PVC, polycarbonate, epoxy resin and molded products).
2 Principles
For the food simulants of food contact materials and products (PVC,
polycarbonate, epoxy resin, and molded products),use liquid chromatography-
mass spectrometry/mass spectrometry to detect; in which, water-based, acidic
food, and alcoholic food simulants directly inject, the oil-based food simulant
inject after being extracted through methanol solution and then use liquid
chromatography-mass spectrometry/mass spectrometry to detect bisphenol A
in food simulants; use the method of external standard peak area to quantify.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are analytical
grade, the water is the grade-1 water specified in GB/T 6682. The containers
and transfer apparatuses in the test shall avoid using plastic materials.
3.1 Reagents
3.1.1 Water-based, acidic, alcoholic, oil-based food simulants. The reagents
used are according to the provisions of GB 5009.156.
4.1.1.1 Standard working solution of water-based, acidic food and
alcoholic food simulants
Accurately PIPETTE 0mL, 0.01mL, 0.05mL, 0.1mL, 0.5mL, 1.0mL of bisphenol
A standard intermediate solution into 10mL volumetric flask; USE water to dilute
it; OBTAIN standard working solution with bisphenol A concentration of
0.00mg/L, 0.01mg/L, 0.05mg/L, 0.1mg/L, 0.5mg/L,1.0mg/L, respectively. In the
same way, USE the corresponding water-based, acidic food and alcoholic food
simulants to prepare bisphenol A standard working solution with the same
concentration series.
4.1.1.2 Oil-based food simulant standard working solution
Respectively WEIGH 1g (accurate to 0.01g) of oil-based food stimulant; PLACE
it into 7 stoppered test tubes; USE micro-scale glass syringe which is calibrated
by gravimetric method to respectively move 0mL, 0.01mL, 0.03mL, 0.05mL,
0.07mL, 0.1mL, 0.3mL of bisphenol A standard intermediate solution into test
tubes; OBTAIN standard working solution with the concentration of 0.00mg/kg,
0.10mg/kg, 0.30mg/kg, 0.50mg/kg, 0.70mg/kg, 1.0mg/kg, 3.0mg/kg,
respectively. ADD respectively 3mL of n-hexane into each tube; MIX it uniformly;
ADD 2mL of methanol-water mixture (1+1); KEEP vortex and vibration for 2 min;
LET it stand for stratification. USE glass syringe to suck up the substratum
aqueous solution; FILTER it through 0.2μm nylon filter membrane for
determination.
4.1.2 Preparation of food simulant test solution
4.1.2.1 General rules
This standard food simulation test uses water-based, acidic food, alcoholic, oil-
based food simulants, which can include water-based, acidic food, alcoholic
food, and fatty food. The required test solution is obtained by migration test and
stored in a refrigerator at 4° C in dark place for a week.
4.1.2.2 Migration test
Note. The actual food simulants and migration conditions refer to the provisions of GB
5009.156.
4.1.2.2.1 Raw materials
Tightly TILE the monolayer of raw material sample on the paper of known size;
CALCULATE its surface area by cuboid (thickness cannot be ignored). For each
0.06dm2 food contact area, 10mL (or 10g) of food simulants is required, PLACE
it at 40°C for 240h ± 0.5h; CONDUCT a migration test (or by weight).
4.1.2.2.2 Molded products
Where.
c - The bisphenol A concentration in food simulant test solution, in milligrams
per liter (mg/L) or milligrams per kilogram (mg/kg);
y - The peak area of bisphenol A in food simulant test solution;
b - The intercept of regression curve;
a - The slope of regression curve.
5.2 Conversion calculation of bisphenol A specific migration quantity
According to the food simulant volume used in migration experiment and the
detection area of test sample and food stimulant, the bisphenol A concentration
in food simulant test solution obtained in 5.1 is calculated through mathematical
conversion to obtain the specific migration quantity of bisphenol A, expressed
in (mg/kg) or (mg/dm2). The specific operation refers to the provisions of GB
5009.156.
The calculation results are expressed as the arithmetic mean of the two
independent determination results obtained under repeatability conditions, and
the results are retained with two significant figures.
6 Precision
The absolute difference between two independent determinations obtained
under repeatability conditions shall not exceed 10% of the arithmetic mean.
7 Others
The method detection limit of bisphenol A in water-based, acidic food and
alcoholic food simulants is 0.001mg/L, and the method detection limit of
bisphenol A in oil-based food simulant is 0.01mg/kg.
The method quantitative limit of bisphenol A in water-based, acidic food and
alcoholic food simulants is 0.01mg/L, and the method quantitative limit of
bisphenol A in oil-based food simulant is 0.10mg/kg.
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GB 31604.10-2016: National Food Safety Standard -- Food Contact Materials and Articles -- Determination of migration of 2,2-bis (4-hydroxyphenyl) propane (bisphenol A)
GB 31604.10-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Food contact materials and products -
Determination of migration quantity of 2,2-bis(4-
hydroxyphenyl) propane (bisphenol A)
食品接触材料及制品
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. MARCH 1, 2017
Issued by. National Health and Family Planning Commission of the PRC
Table of Contents
1 Scope .. 3
2 Principles .. 3
3 Reagents and materials . 3
4 Analytical procedures . 4
5 Analysis results expression . 7
6 Precision . 8
7 Others . 8
Appendix A Reference Mass Spectrometry Conditions . 9
National food safety standard -
Food contact materials and products -
Determination of migration quantity of 2,2-bis(4-
hydroxyphenyl) propane (bisphenol A)
1 Scope
This standard specifies the method for determining bisphenol A migration
quantity in food contact materials and products (PVC, polycarbonate, epoxy
resin and molded products).
This standard applies to liquid chromatography-mass spectrometry/mass
spectrometry detection of bisphenol A migration quantity in food contact
materials and products (PVC, polycarbonate, epoxy resin and molded products).
2 Principles
For the food simulants of food contact materials and products (PVC,
polycarbonate, epoxy resin, and molded products),use liquid chromatography-
mass spectrometry/mass spectrometry to detect; in which, water-based, acidic
food, and alcoholic food simulants directly inject, the oil-based food simulant
inject after being extracted through methanol solution and then use liquid
chromatography-mass spectrometry/mass spectrometry to detect bisphenol A
in food simulants; use the method of external standard peak area to quantify.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are analytical
grade, the water is the grade-1 water specified in GB/T 6682. The containers
and transfer apparatuses in the test shall avoid using plastic materials.
3.1 Reagents
3.1.1 Water-based, acidic, alcoholic, oil-based food simulants. The reagents
used are according to the provisions of GB 5009.156.
4.1.1.1 Standard working solution of water-based, acidic food and
alcoholic food simulants
Accurately PIPETTE 0mL, 0.01mL, 0.05mL, 0.1mL, 0.5mL, 1.0mL of bisphenol
A standard intermediate solution into 10mL volumetric flask; USE water to dilute
it; OBTAIN standard working solution with bisphenol A concentration of
0.00mg/L, 0.01mg/L, 0.05mg/L, 0.1mg/L, 0.5mg/L,1.0mg/L, respectively. In the
same way, USE the corresponding water-based, acidic food and alcoholic food
simulants to prepare bisphenol A standard working solution with the same
concentration series.
4.1.1.2 Oil-based food simulant standard working solution
Respectively WEIGH 1g (accurate to 0.01g) of oil-based food stimulant; PLACE
it into 7 stoppered test tubes; USE micro-scale glass syringe which is calibrated
by gravimetric method to respectively move 0mL, 0.01mL, 0.03mL, 0.05mL,
0.07mL, 0.1mL, 0.3mL of bisphenol A standard intermediate solution into test
tubes; OBTAIN standard working solution with the concentration of 0.00mg/kg,
0.10mg/kg, 0.30mg/kg, 0.50mg/kg, 0.70mg/kg, 1.0mg/kg, 3.0mg/kg,
respectively. ADD respectively 3mL of n-hexane into each tube; MIX it uniformly;
ADD 2mL of methanol-water mixture (1+1); KEEP vortex and vibration for 2 min;
LET it stand for stratification. USE glass syringe to suck up the substratum
aqueous solution; FILTER it through 0.2μm nylon filter membrane for
determination.
4.1.2 Preparation of food simulant test solution
4.1.2.1 General rules
This standard food simulation test uses water-based, acidic food, alcoholic, oil-
based food simulants, which can include water-based, acidic food, alcoholic
food, and fatty food. The required test solution is obtained by migration test and
stored in a refrigerator at 4° C in dark place for a week.
4.1.2.2 Migration test
Note. The actual food simulants and migration conditions refer to the provisions of GB
5009.156.
4.1.2.2.1 Raw materials
Tightly TILE the monolayer of raw material sample on the paper of known size;
CALCULATE its surface area by cuboid (thickness cannot be ignored). For each
0.06dm2 food contact area, 10mL (or 10g) of food simulants is required, PLACE
it at 40°C for 240h ± 0.5h; CONDUCT a migration test (or by weight).
4.1.2.2.2 Molded products
Where.
c - The bisphenol A concentration in food simulant test solution, in milligrams
per liter (mg/L) or milligrams per kilogram (mg/kg);
y - The peak area of bisphenol A in food simulant test solution;
b - The intercept of regression curve;
a - The slope of regression curve.
5.2 Conversion calculation of bisphenol A specific migration quantity
According to the food simulant volume used in migration experiment and the
detection area of test sample and food stimulant, the bisphenol A concentration
in food simulant test solution obtained in 5.1 is calculated through mathematical
conversion to obtain the specific migration quantity of bisphenol A, expressed
in (mg/kg) or (mg/dm2). The specific operation refers to the provisions of GB
5009.156.
The calculation results are expressed as the arithmetic mean of the two
independent determination results obtained under repeatability conditions, and
the results are retained with two significant figures.
6 Precision
The absolute difference between two independent determinations obtained
under repeatability conditions shall not exceed 10% of the arithmetic mean.
7 Others
The method detection limit of bisphenol A in water-based, acidic food and
alcoholic food simulants is 0.001mg/L, and the method detection limit of
bisphenol A in oil-based food simulant is 0.01mg/kg.
The method quantitative limit of bisphenol A in water-based, acidic food and
alcoholic food simulants is 0.01mg/L, and the method quantitative limit of
bisphenol A in oil-based food simulant is 0.10mg/kg.