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GB 31604.54-2023: National food safety standard - Food contact materials and products - Determination of migration of bisphenol F and S
GB 31604.54-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Contact Materials
and Products - Determination of Migration of Bisphenol F
and S
ISSUED ON: SEPTEMBER 6, 2023
IMPLEMENTED ON: MARCH 6, 2024
Issued by: National Health Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope ... 3
Method 1 - Liquid Chromatography ... 3
2 Principle ... 3
3 Reagents and Materials ... 3
4 Instruments and Equipment ... 6
5 Analytical Procedures ... 6
6 Expression of Analysis Results ... 9
7 Precision ... 10
8 Others ... 10
Method 2 - Liquid Chromatography - Tandem Mass Spectrometry ... 11
9 Principle ... 11
10 Reagents and Materials ... 11
11 Instruments and Equipment ... 14
12 Analytical Procedures ... 14
13 Expression of Analysis Results ... 17
14 Precision ... 17
15 Others ... 17
Appendix A Liquid Chromatograms of Bisphenol F and Bisphenol S ... 18
Appendix B Mass Spectrometry Reference Conditions of Liquid Chromatography -
Tandem Mass Spectrometry ... 23
Appendix C Total Ions Chromatograms of Bisphenol F and Bisphenol S ... 24
National Food Safety Standard - Food Contact Materials
and Products - Determination of Migration of Bisphenol F
and S
1 Scope
This Standard specifies the methods for the determination of migration of bisphenol F and S in
food contact materials and products by liquid chromatography and liquid chromatography -
tandem mass spectrometry.
Method 1 - liquid chromatography is applicable to the determination of migration of bisphenol
F and S in plastic materials and products for food contact, paints and coatings for food contact,
paper and cardboard materials and products for food contact.
Method 2 - liquid chromatography - tandem mass spectrometry is applicable to the
determination of migration of bisphenol F and S in food contact materials and products.
Method 1 - Liquid Chromatography
2 Principle
After food contact materials and products are subject to migration test in accordance with GB
31604.1 and GB 5009.156, adopt liquid chromatography for detection. Specifically speaking,
after filtration, aqueous, acidic and alcoholic food simulants are directly injected; use nitrogen
to blow-dry 95% (volume fraction) ethanol, then, use ethanol-water to reach a constant volume,
filter and inject the sample; use methanol-water mixture to extract oily food simulants, filter
and inject the sample; use nitrogen to blow-dry the chemical alternative solvent - isooctane, use
methanol-water to reach a constant volume, filter and inject the sample. Adopt the external
standard method for quantitative determination.
3 Reagents and Materials
Unless it is otherwise specified, the reagents used in this Method are all chromatographically
pure, and the water is Grade-1 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Aqueous, acidic, alcoholic and oily food simulants and chemical alternative solvents: the
reagents used shall comply with the stipulations of GB 5009.156.
3.1.2 n-Hexane (C6H14).
3.1.3 Methanol (CH4O).
3.1.4 Acetonitrile (C2H3N).
3.1.5 Isooctane (C8H18).
3.1.6 Acetone (C3H6O).
3.1.7 Ethanol (C2H6O).
3.1.8 Corn oil: chemically pure, complies with the requirements of GB 5009.156.
3.2 Preparation of Reagents
3.2.1 Aqueous, acidic, alcoholic, corn oil food simulants and chemical alternative solvents:
operate in accordance with GB 5009.156.
3.2.2 Methanol-water mixture (1 + 1): measure-take 100 mL of methanol and 100 mL of water,
and evenly mix it.
3.2.3 Ethanol-water mixture (1 + 1): measure-take 100 mL of ethanol and 100 mL of water, and
evenly mix it.
3.3 Reference Materials
3.3.1 Bisphenol F (C13H12O2, CAS: 620-92-8): purity  99%, or a standard substance certified
by the state and awarded a reference material certificate.
3.3.2 Bisphenol S (C12H10O4S, CAS: 80-09-1): purity  99%, or a standard substance certified
by the state and awarded a reference material certificate.
3.4 Preparation of Standard Solutions
3.4.1 Standard stock solutions
3.4.1.1 Bisphenol F (bisphenol S) standard stock solution A (100 mg/L, methanol)
Accurately weigh-take 10 mg (accurate to 0.1 mg) of bisphenol F (bisphenol S) reference
material, use methanol to dissolve it and reach a constant volume in a 100 mL volumetric flask,
then, evenly mix it. Transfer the solution to a brown standard solution stock bottle and store it
in a refrigerator at 4 C and away from light. It shall remain valid for 3 months.
3.4.1.2 Bisphenol F (bisphenol S) standard stock solution B (100 mg/L, isooctane)
Accurately weigh-take 10 mg (accurate to 0.1 mg) of bisphenol F (bisphenol S) reference
material, use 10 mL of acetone to dissolve it, then, use isooctane to reach a constant volume in
a 100 mL volumetric flask, then, evenly mix it. Transfer the solution to a brown standard
Respectively and accurately add 2 g (accurate to 0.01 g) of corn oil into five 10 mL test tubes
with stoppers, add 200 L, 300 L, 400 L, 1.00 mL and 2.00 mL of bisphenol F standard
intermediate solution C (3.4.2.3); add 600 L of bisphenol S standard intermediate solution D
(3.4.2.4), and 100 L, 200 L, 400 L and 1.00 mL of bisphenol S standard intermediate
solution C (3.4.2.3) to obtain mixed standard solutions with bisphenol F concentration of 100
g/kg, 150 g/kg, 200 g/kg, 500 g/kg and 1.00 mg/kg, and bisphenol S concentration of 30.0
g/kg, 50.0 g/kg, 100 g/kg, 200 g/kg and 500 g/kg. Prepare them right before use.
Respectively add 3 mL of n-hexane to each test tube and evenly mix it. Respectively add 2.20
mL, 2.60 mL, 2.40 mL, 1.60 mL and 0 mL of methanol-water mixture into five 10 mL test tubes
with stoppers; conduct vortex oscillation for 2 min and let it stand for stratification. Draw-take
the lower-layer solution, filter it through a 0.45 m polytetrafluoroethylene microporous filter
membrane, and reserve it for determination.
3.4.3.3 Standard working solutions of chemical alternative solvent - isooctane
Accurately draw-take 0.150 mL, 0.250 mL, 0.500 mL, 2.50 mL and 5.00 mL of bisphenol F
and bisphenol S standard intermediate solution B (3.4.2.2) into five 50 mL volumetric flasks;
use isooctane to reach a constant volume to obtain bisphenol F and bisphenol S mixed standard
working solutions with a concentration of 30.0 g/L, 50.0 g/L, 100 g/L, 500 g/L and 1.00
mg/L. Before injecting into the instrument, it must be handled simultaneously with the food
simulant soaking solution in 5.1.2.4.
4 Instruments and Equipment
4.1 Liquid chromatograph, equipped with ultraviolet detector (UV) or diode array detector
(DAD).
4.2 Vortex oscillator.
4.3 Pipettes: 20 L, 50 L, 250 L, 1,000 L and 5,000 L.
4.4 Analytical balance: with a division value of 0.0001 g and 0.01 g, respectively.
4.5 Constant-temperature water bath.
4.6 Nitrogen blower.
4.7 Polytetrafluoroethylene microporous filter membrane: 0.45 m.
5 Analytical Procedures
5.1 Preparation of Test Solutions
5.1.1 Migration test
In accordance with the requirements of GB 5009.156 and GB 31604.1, conduct a migration test
on the sample to obtain a food simulant test solution. If the test solution obtained from the
migration test cannot be immediately tested, it shall be stored in a refrigerator at 4 C and away
from light. The storage period is 7 days. Before proceeding to the next step of test, the food
simulant test solution shall be returned to room temperature.
5.1.2 Treatment of food simulants
5.1.2.1 Aqueous, acidic and alcoholic [except for 95% (volume fraction) ethanol] food
simulants
Accurately transfer-take about 2 mL of the aqueous, acidic and alcoholic food simulants
obtained from the migration test, use a 0.45 m polytetrafluoroethylene microporous filter
membrane to filter it, and reserve it for determination.
5.1.2.2 95% (volume fraction) ethanol
Accurately draw-take 1 mL of 95% (volume fraction) ethanol obtained from the migration test
into a test tube and use nitrogen to blow-dry it. Accurately add 1 mL of ethanol-water mixture
into the test tube and conduct vortex mixing for 2 min. Use a 0.45 m polytetrafluoroethylene
microporous filter membrane to filter the solution, and reserve it for determination.
5.1.2.3 Oily food simulants
Accurately weigh-take 2 g (accurate to 0.01 g) of corn oil obtained from the migration test into
a 10 mL test tube, add 3 mL of n-hexane and evenly mix it. Add 3 mL methanol-water mixture,
conduct vortex oscillation for 2 min, and let it stand for stratification. Draw-take the lower-
layer solution, filter it through a 0.45 m polytetrafluoroethylene microporous filter membrane,
and reserve it for determination.
5.1.2.4 Chemical alternative solvent - isooctane
Accurately draw-take 5 mL of chemical alternative solvent - isooctane obtained from the
migration test into a test tube and use nitrogen to blow-dry it. Accurately add 5 mL of methanol-
water mixture into the test tube and conduct vortex mixing for 2 min. Use a 0.45 m
polytetrafluoroethylene microporous filter membrane to filter the solution, and reserve it for
determination.
5.1.3 Preparation of blank test solution
In accordance with 5.1.1 and 5.1.2, handle the food simulants and chemical alternative solvents
not in contact with food contact materials and products.
5.2 Reference Conditions of Instrument
The reference conditions of the instrument are as follows:
a) Chromatographic column: C18 column, column length 150 mm, inner diameter 4.6
mm, particle size 5 m; or one with equivalent performance.
oily food simulants, the detection limit of bisphenol F in food contact materials and products is
0.03 mg/kg and the quantification limit is 0.1 mg/kg; the detection limit of bisphenol S is 0.01
mg/kg and the quantification limit is 0.03 mg/kg.
Method 2 - Liquid Chromatography - Tandem Mass
Spectrometry
9 Principle
After food contact materials and products are subject to migration test in accordance with GB
31604.1 and GB 5009.156, adopt liquid chromatography - tandem mass spectrometry for
detection. Specifically speaking, after filtration, aqueous, acidic and alcoholic food simulants
are directly injected; oily food simulants are extracted through methanol-water mixture, filtered,
then injected. Use nitrogen to blow-dry chemical alternative solvent - isooctane, then, use
methanol-water to reach a constant volume, filter and inject the sample. Adopt the external
standard method for quantitative determination.
10 Reagents and Materials
Unless it is otherwise specified, the reagents used in this Method are all chromatographically
pure, and the water is Grade-1 water specified in GB/T 6682.
10.1 Reagents
10.1.1 Aqueous, acidic, alcoholic and oily food simulants and chemical alternative solvents: the
reagents used shall comply with the stipulations of GB 5009.156.
10.1.2 n-Hexane (C6H14).
10.1.3 Methanol (CH4O).
10.1.4 Isooctane (C8H18).
10.1.5 Acetone (C3H6O).
10.1.6 Olive oil: chemically pure, complies with the requirements of GB 5009.156.
10.2 Preparation of Reagents
10.2.1 Aqueous, acidic, alcoholic, olive oil food simulants and chemical alternative solvents:
operate in accordance with GB 5009.156.
10.2.2 Methanol-water mixture (1 + 1): measure-take 100 mL of methanol and 100 mL of water,
and evenly mix it.
10.3 Reference Materials
Same as 3.3.
10.4 Preparation of Standard Solutions
10.4.1 Standard stock solutions
10.4.1.1 Bisphenol F standard stock solution A (1,000 mg/L, methanol)
Accurately weigh-take 50 mg (accurate to 0.1 mg) of bisphenol F reference material, use
methanol to dissolve it and reach a constant volume in a 50 mL volumetric flask, then, evenly
mix it. Transfer the solution to a brown standard solution stock bottle and store it in a
refrigerator at 4 C and away from light. It shall remain valid for 3 months.
10.4.1.2 Bisphenol S standard stock solution A (50 mg/L, methanol)
Accurately weigh-take 10 mg (accurate to 0.1 mg) of bisphenol S reference material, use
methanol to dissolve it and reach a constant volume in a 200 mL volumetric flask, then, evenly
mix it. Transfer the solution to a brown standard solution stock bottle and store it in a
refrigerator at 4 C and away from light. It shall remain valid for 3 months.
10.4.1.3 Bisphenol F standard stock solution B (1,000 mg/L, isooctane)
Accurately weigh-take 50 mg (accurate to 0.1 mg) of bisphenol F reference material, add 10
mL of acetone to dissolve it, then, use isooctane to reach a constant volume in a 50 mL
volumetric flask, then, evenly mix it. Transfer the solution to a brown standard solution stock
bottle and store it in a refrigerator at 4 C and away from light. It shall remain valid for 3 months.
10.4.1.4 Bisphenol S standard stock solution B (50 mg/L, isooctane)
Accurately weigh-take 10 mg (accurate to 0.1 mg) of bisphenol S reference material, add 10
mL of acetone to dissolve it, then, use isooctane to reach a constant volume in a 200 mL
volumetric flask, then, evenly mix it. Transfer the solution to a brown standard solution stock
bottle and store it in a refrigerator at 4 C and away from light. It shall remain valid for 3 months.
10.4.2 Standard intermediate solutions
10.4.2.1 Bisphenol F and bisphenol S standard intermediate solution A (10 mg/L, 0.5 mg/L,
methanol)
Accurately draw-take 1.00 mL of bisphenol F standard stock solution A (10.4.1.1) and 1.00 mL
of bisphenol S standard stock solution A (10.4.1.2) into a 100 mL volumetric flask, use
methanol to reach a constant volume, then, evenly mix it. Transfer the solution to a brown
standard solution stock bottle and store it in a refrigerator at 4 C and away from light. It shall
remain valid for 1 month.
10.4.2.2 Bisphenol F and bisphenol S standard intermediate solution B (10 mg/L, 0.5 mg/L,
isooctane)
Accurately 1.00 mL of bisphenol F standard stock solution B (10.4.1.3) and 1.00 mL of
bisphenol S standard stock solution B (10.4.1.4) into a 100 mL volumetric flask, use isooctane
to reach a constant volu...