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GB 31604.57-2023 English PDF (GB31604.57-2023)
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GB 31604.57-2023: National food safety standard - Food contact materials and products - Determination of migration of benzophenone substances
GB 31604.57-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Contact Materials
and Products - Determination of Migration of Benzophenone
Substances
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 ... 4
4 Instruments and Equipment ... 6
5 Analytical Procedures ... 7
6 Expression of Analysis Results ... 9
7 Precision ... 11
8 Others ... 11
Method 2 - Liquid Chromatography - Tandem Mass Spectrometry ... 12
9 Principle ... 12
10 Reagents and Materials ... 12
11 Instruments and Equipment ... 15
12 Analytical Procedures ... 15
13 Expression of Analysis Results ... 18
14 Precision ... 18
15 Others ... 18
Appendix A Liquid Chromatograms of Standard Solutions of Eight Benzophenones 20
Appendix B Mass Spectrometry Reference Conditions ... 23
Appendix C Liquid Chromatograph - Tandem Mass Spectrometer Total Ions (TIC)
Chromatograms of Eight Benzophenones ... 24
National Food Safety Standard - Food Contact Materials
and Products - Determination of Migration of Benzophenone
Substances
1 Scope
This Standard specifies the methods for the determination of migration of eight benzophenone
substances in food contact materials and products.
Method 1 - liquid chromatography is applicable to the determination of migration of (2-
hydroxy-4-methoxyphenyl) (2-hydroxyphenyl) ketone, 2,4-dihydroxybenzophenone, (2-
hydroxy-4-methoxyphenyl) phenyl ketone, 4-4-dihydroxybenzophenone, 2-hydroxy-4-n-
octoxy-benzophenone, 2-hydroxy-4-n-hexyloxy-benzophenone, benzophenone and 4-4-
difluoro-benzophenone in plastics, paints and coatings, rubber, and food contact materials and
products using inks in water, 4% (volume fraction) acetic acid, 10% (volume fraction) ethanol,
20% (volume fraction) ethanol, 50% (volume fraction) ethanol food simulants, as well as
chemical alternative solvents - 95% (volume fraction) ethanol and isooctane.
Method 2 - liquid chromatography - tandem mass spectrometry is applicable to the
determination of migration of (2-hydroxy-4-methoxyphenyl) (2-hydroxyphenyl) ketone, 2,4-
dihydroxybenzophenone, (2-hydroxy-4-methoxyphenyl) phenyl ketone, 4-4-
dihydroxybenzophenone, 2-hydroxy-4-n-octoxy-benzophenone, 2-hydroxy-4-n-hexyloxy-
benzophenone, benzophenone and 4-4-difluoro-benzophenone in plastics, paints and coatings,
rubber, and food contact materials and products using inks in water, 4% (volume fraction) acetic
acid, 10% (volume fraction) ethanol, 20% (volume fraction) ethanol, 50% (volume fraction)
ethanol and olive oil food simulants, as well as chemical alternative solvents - 95% (volume
fraction) ethanol and isooctane.
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. Water, 4% (volume
fraction) acetic acid, 10% (volume fraction) ethanol, 20% (volume fraction) ethanol and 50%
(volume fraction) ethanol food simulants are directly injected; chemical alternative solvent -
95% (volume fraction) ethanol is diluted by water, filtered, then, injected. Use nitrogen to blow
the chemical alternative solvent - isooctane, then, use methanol-water to re-dissolve it, filter,
then, inject the sample. Adopt the external standard method of peak area for quantitative
determination.
3 Reagents and Materials
Unless it is otherwise specified, the reagents used in this Method are all analytically pure, and
the water is Grade-1 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Glacial acetic acid (CH3COOH).
3.1.2 Absolute ethanol (C2H5OH).
3.1.3 Isooctane (C8H18).
3.1.4 Methanol (CH3OH): chromatographically pure.
3.1.5 Dimethyl sulfoxide (C2H6OS).
3.2 Preparation of Reagents
3.2.1 4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20%
(volume fraction) ethanol solution and 50% (volume fraction) ethanol solution are prepared in
accordance with GB 5009.156.
3.2.2 95% (volume fraction) ethanol solution: evenly mix absolute ethanol and water in a
volume ratio of 95 : 5.
3.2.3 Methanol-water solution (7 + 3): evenly mix methanol and water in a volume ratio of 7 :
3.
3.3 Reference Materials
3.3.1 (2-hydroxy-4-methoxyphenyl) (2-hydroxyphenyl) ketone (C14H12O4, CAS: 131-53-3):
purity 98%, or a standard substance certified by the state and awarded a reference material
certificate.
3.3.2 2,4-dihydroxybenzophenone (C13H10O3, CAS: 131-56-6): purity 98%, or a standard
substance certified by the state and awarded a reference material certificate.
3.3.3 (2-hydroxy-4-methoxyphenyl) phenyl ketone (C14H12O3, CAS: 131-57-7): purity 98%,
or a standard substance certified by the state and awarded a reference material certificate.
3.3.4 4-4-dihydroxybenzophenone (C13H10O3, CAS: 611-99-4): purity 98%, or a standard
substance certified by the state and awarded a reference material certificate.
3.3.5 2-hydroxy-4-n-octoxy-benzophenone (C21H26O3, CAS: 1843-05-6): purity 98%, or a
standard substance certified by the state and awarded a reference material certificate.
3.3.6 2-hydroxy-4-n-hexyloxy-benzophenone (C19H22O3, CAS: 3293-97-8): purity 98%, or a
standard substance certified by the state and awarded a reference material certificate.
3.3.7 Benzophenone (C13H10O, CAS: 119-61-9): purity 98%, or a standard substance certified
by the state and awarded a reference material certificate.
3.3.8 4-4-difluoro-benzophenone (C13H8F2O, CAS: 345-92-6): purity 98%, 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 (1,000 mg/L)
Accurately weigh-take 50 mg (accurate to 0.1 mg) of each of the eight benzophenone reference
materials, respectively use methanol to dissolve them, then, transfer them to eight 50 mL
volumetric flasks. Use methanol to reach a constant volume to the scale and evenly mix them.
Transfer the solutions to brown glass containers and store them airtight at 4 C away from light.
They shall remain valid for 6 months.
3.4.2 Standard mixed intermediate solution
Respectively draw-take 0.5 mL of 4-4-dihydroxybenzophenone, benzophenone and 4-4-
difluoro-benzophenone standard stock solutions (1,000 mg/L) and 2.0 mL of the standard stock
solutions (1,000 mg/L) of the other five benzophenone substances into a 100 mL volumetric
flask. Use methanol to reach a constant volume to the scale, evenly mix it to obtain a Standard
mixed intermediate solution, in which, the concentration of 4-4-dihydroxybenzophenone,
benzophenone and 4-4-difluoro-benzophenone is 5.0 mg/L, and the concentration of the other
five benzophenone substances is 20.0 mg/L. Transfer the solution to a brown glass container
and store it airtight at 4 C away from light. It shall remain valid for 3 months.
3.4.3 Standard mixed series of working solutions
3.4.3.1 Standard mixed series of working solutions of water, 4% (volume fraction) acetic
acid, 10% (volume fraction) ethanol, 20% (volume fraction) ethanol and 50% (volume
fraction) ethanol
Respectively draw-take 40 L, 100 L, 200 L, 400 L and 600 L of the standard mixed
intermediate solution into ...
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GB 31604.57-2023: National food safety standard - Food contact materials and products - Determination of migration of benzophenone substances
GB 31604.57-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Contact Materials
and Products - Determination of Migration of Benzophenone
Substances
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 ... 4
4 Instruments and Equipment ... 6
5 Analytical Procedures ... 7
6 Expression of Analysis Results ... 9
7 Precision ... 11
8 Others ... 11
Method 2 - Liquid Chromatography - Tandem Mass Spectrometry ... 12
9 Principle ... 12
10 Reagents and Materials ... 12
11 Instruments and Equipment ... 15
12 Analytical Procedures ... 15
13 Expression of Analysis Results ... 18
14 Precision ... 18
15 Others ... 18
Appendix A Liquid Chromatograms of Standard Solutions of Eight Benzophenones 20
Appendix B Mass Spectrometry Reference Conditions ... 23
Appendix C Liquid Chromatograph - Tandem Mass Spectrometer Total Ions (TIC)
Chromatograms of Eight Benzophenones ... 24
National Food Safety Standard - Food Contact Materials
and Products - Determination of Migration of Benzophenone
Substances
1 Scope
This Standard specifies the methods for the determination of migration of eight benzophenone
substances in food contact materials and products.
Method 1 - liquid chromatography is applicable to the determination of migration of (2-
hydroxy-4-methoxyphenyl) (2-hydroxyphenyl) ketone, 2,4-dihydroxybenzophenone, (2-
hydroxy-4-methoxyphenyl) phenyl ketone, 4-4-dihydroxybenzophenone, 2-hydroxy-4-n-
octoxy-benzophenone, 2-hydroxy-4-n-hexyloxy-benzophenone, benzophenone and 4-4-
difluoro-benzophenone in plastics, paints and coatings, rubber, and food contact materials and
products using inks in water, 4% (volume fraction) acetic acid, 10% (volume fraction) ethanol,
20% (volume fraction) ethanol, 50% (volume fraction) ethanol food simulants, as well as
chemical alternative solvents - 95% (volume fraction) ethanol and isooctane.
Method 2 - liquid chromatography - tandem mass spectrometry is applicable to the
determination of migration of (2-hydroxy-4-methoxyphenyl) (2-hydroxyphenyl) ketone, 2,4-
dihydroxybenzophenone, (2-hydroxy-4-methoxyphenyl) phenyl ketone, 4-4-
dihydroxybenzophenone, 2-hydroxy-4-n-octoxy-benzophenone, 2-hydroxy-4-n-hexyloxy-
benzophenone, benzophenone and 4-4-difluoro-benzophenone in plastics, paints and coatings,
rubber, and food contact materials and products using inks in water, 4% (volume fraction) acetic
acid, 10% (volume fraction) ethanol, 20% (volume fraction) ethanol, 50% (volume fraction)
ethanol and olive oil food simulants, as well as chemical alternative solvents - 95% (volume
fraction) ethanol and isooctane.
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. Water, 4% (volume
fraction) acetic acid, 10% (volume fraction) ethanol, 20% (volume fraction) ethanol and 50%
(volume fraction) ethanol food simulants are directly injected; chemical alternative solvent -
95% (volume fraction) ethanol is diluted by water, filtered, then, injected. Use nitrogen to blow
the chemical alternative solvent - isooctane, then, use methanol-water to re-dissolve it, filter,
then, inject the sample. Adopt the external standard method of peak area for quantitative
determination.
3 Reagents and Materials
Unless it is otherwise specified, the reagents used in this Method are all analytically pure, and
the water is Grade-1 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Glacial acetic acid (CH3COOH).
3.1.2 Absolute ethanol (C2H5OH).
3.1.3 Isooctane (C8H18).
3.1.4 Methanol (CH3OH): chromatographically pure.
3.1.5 Dimethyl sulfoxide (C2H6OS).
3.2 Preparation of Reagents
3.2.1 4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20%
(volume fraction) ethanol solution and 50% (volume fraction) ethanol solution are prepared in
accordance with GB 5009.156.
3.2.2 95% (volume fraction) ethanol solution: evenly mix absolute ethanol and water in a
volume ratio of 95 : 5.
3.2.3 Methanol-water solution (7 + 3): evenly mix methanol and water in a volume ratio of 7 :
3.
3.3 Reference Materials
3.3.1 (2-hydroxy-4-methoxyphenyl) (2-hydroxyphenyl) ketone (C14H12O4, CAS: 131-53-3):
purity 98%, or a standard substance certified by the state and awarded a reference material
certificate.
3.3.2 2,4-dihydroxybenzophenone (C13H10O3, CAS: 131-56-6): purity 98%, or a standard
substance certified by the state and awarded a reference material certificate.
3.3.3 (2-hydroxy-4-methoxyphenyl) phenyl ketone (C14H12O3, CAS: 131-57-7): purity 98%,
or a standard substance certified by the state and awarded a reference material certificate.
3.3.4 4-4-dihydroxybenzophenone (C13H10O3, CAS: 611-99-4): purity 98%, or a standard
substance certified by the state and awarded a reference material certificate.
3.3.5 2-hydroxy-4-n-octoxy-benzophenone (C21H26O3, CAS: 1843-05-6): purity 98%, or a
standard substance certified by the state and awarded a reference material certificate.
3.3.6 2-hydroxy-4-n-hexyloxy-benzophenone (C19H22O3, CAS: 3293-97-8): purity 98%, or a
standard substance certified by the state and awarded a reference material certificate.
3.3.7 Benzophenone (C13H10O, CAS: 119-61-9): purity 98%, or a standard substance certified
by the state and awarded a reference material certificate.
3.3.8 4-4-difluoro-benzophenone (C13H8F2O, CAS: 345-92-6): purity 98%, 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 (1,000 mg/L)
Accurately weigh-take 50 mg (accurate to 0.1 mg) of each of the eight benzophenone reference
materials, respectively use methanol to dissolve them, then, transfer them to eight 50 mL
volumetric flasks. Use methanol to reach a constant volume to the scale and evenly mix them.
Transfer the solutions to brown glass containers and store them airtight at 4 C away from light.
They shall remain valid for 6 months.
3.4.2 Standard mixed intermediate solution
Respectively draw-take 0.5 mL of 4-4-dihydroxybenzophenone, benzophenone and 4-4-
difluoro-benzophenone standard stock solutions (1,000 mg/L) and 2.0 mL of the standard stock
solutions (1,000 mg/L) of the other five benzophenone substances into a 100 mL volumetric
flask. Use methanol to reach a constant volume to the scale, evenly mix it to obtain a Standard
mixed intermediate solution, in which, the concentration of 4-4-dihydroxybenzophenone,
benzophenone and 4-4-difluoro-benzophenone is 5.0 mg/L, and the concentration of the other
five benzophenone substances is 20.0 mg/L. Transfer the solution to a brown glass container
and store it airtight at 4 C away from light. It shall remain valid for 3 months.
3.4.3 Standard mixed series of working solutions
3.4.3.1 Standard mixed series of working solutions of water, 4% (volume fraction) acetic
acid, 10% (volume fraction) ethanol, 20% (volume fraction) ethanol and 50% (volume
fraction) ethanol
Respectively draw-take 40 L, 100 L, 200 L, 400 L and 600 L of the standard mixed
intermediate solution into ...
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