National Health Commission and State Administration for Market Regulation
Issued on:
2020-09-11
Implemented on:
2021-3-11
Status:
valid
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English
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3500 words
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Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
National food safety standard
Food contact materials and articles
Determination of nonylphenol migration
1 Scope
This standard specifies the determination of nonylphenol migration in food contact materials and articles by liquid chromatography-mass spectrometry/mass spectrometry method.
This standard is applicable to the determination of nonylphenol in soaking solution obtained by migration test on food contact materials and articles which use water, 4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20% (volume fraction) ethanol solution, 50% (volume fraction) ethanol solution, olive oil and 95% (volume fraction) ethanol solution as food simulants respectively or use 95% (volume fraction) ethanol solution and isooctane chemical alternative solvent.
2 Principle
For 4% (volume fraction) acetic acid solution as food simulant, determination is carried out on the sample from the soaking solution obtained by migration test on 4% (volume fraction) acetic acid and neutralized with ammonia water; for olive oil as food simulant, determination is carried out on the sample from the soaking solution obtained by migration test on olive oil and extracted with acetonitrile and purified with n-hexane; for isooctane as chemical alternative solvent, determination is carried out on the sample from the soaking solution obtained by migration test on isooctane and evaporated to dryness, then redissolved with methanol; for other solutions or chemical alternative solvent, determination is directly carried out on the soaking solutions obtained by migration test. The nonylphenol in soaking solution is determined by liquid chromatography-mass spectrometry/mass spectrometry method and quantified by external standard method.
3 Reagents and materials
Unless otherwise specified, analytically-pure reagents and Class-I water specified in GB/T 6682 are adopted for the purpose of this method.
3.1 Reagents
3.1.1 Glacial acetic acid (C2H4O2).
3.1.2 Anhydrous ethanol (C2H6O).
3.1.3 95% ethanol.
3.1.4 Isooctane (C8H18).
3.1.5 Olive oil: chemically pure, complying with GB 5009.156.
3.1.6 Methanol (CH4O): chromatographically pure.
3.1.7 Acetonitrile (C2H3N): chromatographically pure.
3.1.8 N-hexane (C6H14).
3.1.9 Ammonia water: chromatographic purity, with a volume fraction ≥25%.
3.2 Preparation of reagents
4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20% (volume fraction) ethanol solution and 50% (volume fraction) ethanol solution are prepared according to GB 5009.156.
3.3 Standards
Nonylphenol (mixture of branched isomers, C15H24O, CAS No.: 84852-15-3) standard solution: 1,000mg/L
3.4 Preparation of standard solutions
3.4.1 Standard intermediate solution (100mg/L)
Accurately transfer 1.00mL nonylphenol standard solution (1,000mg/L) into a 10mL volumetric flask, dilute to the scale with methanol, and then mix well. The solution is valid for 6 months in the refrigerator at 0℃~4℃.
3.4.2 Standard intermediate solution (5mg/L)
Accurately transfer 0.50mL nonylphenol standard intermediate solution (100mg/L) into a 10mL volumetric flask, dilute to the scale with methanol, and then mix well.
3.4.3 Standard working solutions
3.4.3.1 4% (volume fraction) acetic acid standard working solution
Accurately transfer 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL and 0.40mL standard intermediate solutions (5mg/L) into six 10mL volumetric flasks respectively, and dilute to the scale with 4% (volume fraction) acetic acid solution. The standard working solutions with mass concentrations of 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L and 0.20mg/L are obtained. Prior to practice, the solutions shall be treated synchronously with food simulant soaking solution according to 5.1.2.1.
3.4.3.2 Oil-based food simulant standard working solution
Accurately weigh 5.00g (accurate to 0.1mg) olive oil into six glass centrifuge tubes with stoppers respectively, add 0.01mL, 0.02mL, 0.03mL, 0.05mL, 0.10mL and 0.20mL standard intermediate solutions (5mg/L) respectively, vortex for mixing well to obtain 0.01mg/kg, 0.02mg/kg, 0.03mg/kg, 0.05mg/kg, 0.10mg/kg and 0.20mg/kg standard working solutions. Prior to practice, the solutions shall be treated synchronously with food simulant soaking solution according to 5.1.2.2.
3.4.3.3 Isooctane standard working solution
Accurately transfer 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL and 0.40mL standard intermediate solutions (5mg/L) into six 10mL volumetric flasks respectively, dilute to the scale with isooctane, and mix well to obtain the standard working solutions with mass concentrations of 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L and 0.20mg/L respectively. Prior to practice, the solutions shall be treated synchronously with food simulant soaking solution according to 5.1.2.3.
3.4.3.4 Other food simulant and chemical alternative solvent standard working solutions
Accurately pipet 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL and 0.40mL standard intermediate solutions (5mg/L) into six 10mL volumetric flasks respectively, dilute to the scale with corresponding food simulant or chemical alternative solvent to obtain other water-based food simulant or chemical alternative solvent standard working solutions with mass concentrations of 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L and 0.20mg/L respectively.
4 Apparatus
4.1 Liquid chromatography-tandem triple quadrupole mass spectrometer: equipped with electrospray ionization (ESI).
4.2 Vortex oscillator.
4.3 Analytical balances: with sensibility of 0.0001g and 0.01g respectively.
4.4 High-speed centrifuge: with a maximum rotation speed ≥10,000r/min.
5 Analysis steps
5.1 Preparation of test solution
5.1.1 Migration test
Food contact materials and articles are subjected to migration test according to the requirements of GB 31604.1 and GB 5009.156. The soaking solution obtained by migration test shall be stored in a refrigerator at 4℃ free from light if cannot be tested immediately. The soaking solution shall be restored to room temperature before the next test.
5.1.2 Treatment of soaking solution
5.1.2.1 Treatment of 4% (volume fraction) acetic acid soaking solution
Transfer 5.0mL 4% (volume fraction) acetic acid soaking solution obtained by migration test, add 0.5mL ammonia water, mix well, centrifuge for 5min at 10,000r/min, and the supernatant is to be determined.
5.1.2.2 Treatment of oil-based food simulants
Weigh 5.00g (accurate to 0.01g) olive oil soaking solution obtained by migration test into a glass centrifuge tube with stopper, add 2mL n-hexane, mix well, then add 5.0mL acetonitrile, vortex for oscillating for 0.5min, centrifuge for 5min at 4,000r/min, take the upper acetonitrile solution for centrifuging at 10,000r/min for 5min, and the supernatant is to be determined.
5.1.2.3 Treatment of isooctane soaking solution
Transfer 10.0mL isooctane soaking solution obtained by migration test, evaporate to nearly dry at 40℃ in a rotary way, accurately transfer 10.0mL dissolved methanol residue, centrifuge for 5min at 10,000r/min , and the supernatant is to be determined.
5.1.2.4 Treatment of other food simulant soaking solutions and chemical alternative solvent soaking solutions
Transfer a proper amount of soaking solution obtained by migration test, centrifuge for 5min at 10,000r/min, and the supernatant is to be determined.
5.1.3 Preparation of blank test solution
Treat the food simulants and chemical alternative solvents that are not in contact with food contact materials and articles according to 5.1.1 and 5.1.2.
5.2 Instrument reference conditions
5.2.1 Liquid chromatography conditions
The liquid chromatography reference conditions are as follows:
a) Chromatographic column: C18 column, 2.6μm, 2.1mm×150mm (or equivalent).
b) Mobile phase: methanol-water (90+10, volume ratio).
c) Flow rate: 0.3mL/min.
d) Column temperature: 40℃.
e) Injection volume: 2μL.
5.2.2 Mass spectrometry conditions
The mass spectrometry reference conditions are as follows:
a) Ionization mode: electrospray ionization in negative ion mode (ESI-).
b) Scanning mode of mass spectrometry: multi-reaction monitoring (MRM).
c) See Table A.1 for other mass spectrometry parameters.
5.3 Plotting of standard curve
Determine the standard working solution according to the instrument reference conditions listed in 5.2, plot the standard curve with the concentration of nonylphenol in the standard working solution as X-coordinate and the corresponding quantitative ion peak area as Y-coordinate, and obtain the linear equation. See Annex B for the chromatogram of nonylphenol standard working solution.
1 Scope
2 Principle
3 Reagents and materials
4 Apparatus
5 Analysis steps
6 Expression of analysis results
7 Precision
8 Others
Annex A Reference mass spectrometry conditions
Annex B MRM chromatogram of nonylphenol standard working solution
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
National food safety standard
Food contact materials and articles
Determination of nonylphenol migration
1 Scope
This standard specifies the determination of nonylphenol migration in food contact materials and articles by liquid chromatography-mass spectrometry/mass spectrometry method.
This standard is applicable to the determination of nonylphenol in soaking solution obtained by migration test on food contact materials and articles which use water, 4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20% (volume fraction) ethanol solution, 50% (volume fraction) ethanol solution, olive oil and 95% (volume fraction) ethanol solution as food simulants respectively or use 95% (volume fraction) ethanol solution and isooctane chemical alternative solvent.
2 Principle
For 4% (volume fraction) acetic acid solution as food simulant, determination is carried out on the sample from the soaking solution obtained by migration test on 4% (volume fraction) acetic acid and neutralized with ammonia water; for olive oil as food simulant, determination is carried out on the sample from the soaking solution obtained by migration test on olive oil and extracted with acetonitrile and purified with n-hexane; for isooctane as chemical alternative solvent, determination is carried out on the sample from the soaking solution obtained by migration test on isooctane and evaporated to dryness, then redissolved with methanol; for other solutions or chemical alternative solvent, determination is directly carried out on the soaking solutions obtained by migration test. The nonylphenol in soaking solution is determined by liquid chromatography-mass spectrometry/mass spectrometry method and quantified by external standard method.
3 Reagents and materials
Unless otherwise specified, analytically-pure reagents and Class-I water specified in GB/T 6682 are adopted for the purpose of this method.
3.1 Reagents
3.1.1 Glacial acetic acid (C2H4O2).
3.1.2 Anhydrous ethanol (C2H6O).
3.1.3 95% ethanol.
3.1.4 Isooctane (C8H18).
3.1.5 Olive oil: chemically pure, complying with GB 5009.156.
3.1.6 Methanol (CH4O): chromatographically pure.
3.1.7 Acetonitrile (C2H3N): chromatographically pure.
3.1.8 N-hexane (C6H14).
3.1.9 Ammonia water: chromatographic purity, with a volume fraction ≥25%.
3.2 Preparation of reagents
4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20% (volume fraction) ethanol solution and 50% (volume fraction) ethanol solution are prepared according to GB 5009.156.
3.3 Standards
Nonylphenol (mixture of branched isomers, C15H24O, CAS No.: 84852-15-3) standard solution: 1,000mg/L
3.4 Preparation of standard solutions
3.4.1 Standard intermediate solution (100mg/L)
Accurately transfer 1.00mL nonylphenol standard solution (1,000mg/L) into a 10mL volumetric flask, dilute to the scale with methanol, and then mix well. The solution is valid for 6 months in the refrigerator at 0℃~4℃.
3.4.2 Standard intermediate solution (5mg/L)
Accurately transfer 0.50mL nonylphenol standard intermediate solution (100mg/L) into a 10mL volumetric flask, dilute to the scale with methanol, and then mix well.
3.4.3 Standard working solutions
3.4.3.1 4% (volume fraction) acetic acid standard working solution
Accurately transfer 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL and 0.40mL standard intermediate solutions (5mg/L) into six 10mL volumetric flasks respectively, and dilute to the scale with 4% (volume fraction) acetic acid solution. The standard working solutions with mass concentrations of 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L and 0.20mg/L are obtained. Prior to practice, the solutions shall be treated synchronously with food simulant soaking solution according to 5.1.2.1.
3.4.3.2 Oil-based food simulant standard working solution
Accurately weigh 5.00g (accurate to 0.1mg) olive oil into six glass centrifuge tubes with stoppers respectively, add 0.01mL, 0.02mL, 0.03mL, 0.05mL, 0.10mL and 0.20mL standard intermediate solutions (5mg/L) respectively, vortex for mixing well to obtain 0.01mg/kg, 0.02mg/kg, 0.03mg/kg, 0.05mg/kg, 0.10mg/kg and 0.20mg/kg standard working solutions. Prior to practice, the solutions shall be treated synchronously with food simulant soaking solution according to 5.1.2.2.
3.4.3.3 Isooctane standard working solution
Accurately transfer 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL and 0.40mL standard intermediate solutions (5mg/L) into six 10mL volumetric flasks respectively, dilute to the scale with isooctane, and mix well to obtain the standard working solutions with mass concentrations of 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L and 0.20mg/L respectively. Prior to practice, the solutions shall be treated synchronously with food simulant soaking solution according to 5.1.2.3.
3.4.3.4 Other food simulant and chemical alternative solvent standard working solutions
Accurately pipet 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL and 0.40mL standard intermediate solutions (5mg/L) into six 10mL volumetric flasks respectively, dilute to the scale with corresponding food simulant or chemical alternative solvent to obtain other water-based food simulant or chemical alternative solvent standard working solutions with mass concentrations of 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L and 0.20mg/L respectively.
4 Apparatus
4.1 Liquid chromatography-tandem triple quadrupole mass spectrometer: equipped with electrospray ionization (ESI).
4.2 Vortex oscillator.
4.3 Analytical balances: with sensibility of 0.0001g and 0.01g respectively.
4.4 High-speed centrifuge: with a maximum rotation speed ≥10,000r/min.
5 Analysis steps
5.1 Preparation of test solution
5.1.1 Migration test
Food contact materials and articles are subjected to migration test according to the requirements of GB 31604.1 and GB 5009.156. The soaking solution obtained by migration test shall be stored in a refrigerator at 4℃ free from light if cannot be tested immediately. The soaking solution shall be restored to room temperature before the next test.
5.1.2 Treatment of soaking solution
5.1.2.1 Treatment of 4% (volume fraction) acetic acid soaking solution
Transfer 5.0mL 4% (volume fraction) acetic acid soaking solution obtained by migration test, add 0.5mL ammonia water, mix well, centrifuge for 5min at 10,000r/min, and the supernatant is to be determined.
5.1.2.2 Treatment of oil-based food simulants
Weigh 5.00g (accurate to 0.01g) olive oil soaking solution obtained by migration test into a glass centrifuge tube with stopper, add 2mL n-hexane, mix well, then add 5.0mL acetonitrile, vortex for oscillating for 0.5min, centrifuge for 5min at 4,000r/min, take the upper acetonitrile solution for centrifuging at 10,000r/min for 5min, and the supernatant is to be determined.
5.1.2.3 Treatment of isooctane soaking solution
Transfer 10.0mL isooctane soaking solution obtained by migration test, evaporate to nearly dry at 40℃ in a rotary way, accurately transfer 10.0mL dissolved methanol residue, centrifuge for 5min at 10,000r/min , and the supernatant is to be determined.
5.1.2.4 Treatment of other food simulant soaking solutions and chemical alternative solvent soaking solutions
Transfer a proper amount of soaking solution obtained by migration test, centrifuge for 5min at 10,000r/min, and the supernatant is to be determined.
5.1.3 Preparation of blank test solution
Treat the food simulants and chemical alternative solvents that are not in contact with food contact materials and articles according to 5.1.1 and 5.1.2.
5.2 Instrument reference conditions
5.2.1 Liquid chromatography conditions
The liquid chromatography reference conditions are as follows:
a) Chromatographic column: C18 column, 2.6μm, 2.1mm×150mm (or equivalent).
b) Mobile phase: methanol-water (90+10, volume ratio).
c) Flow rate: 0.3mL/min.
d) Column temperature: 40℃.
e) Injection volume: 2μL.
5.2.2 Mass spectrometry conditions
The mass spectrometry reference conditions are as follows:
a) Ionization mode: electrospray ionization in negative ion mode (ESI-).
b) Scanning mode of mass spectrometry: multi-reaction monitoring (MRM).
c) See Table A.1 for other mass spectrometry parameters.
5.3 Plotting of standard curve
Determine the standard working solution according to the instrument reference conditions listed in 5.2, plot the standard curve with the concentration of nonylphenol in the standard working solution as X-coordinate and the corresponding quantitative ion peak area as Y-coordinate, and obtain the linear equation. See Annex B for the chromatogram of nonylphenol standard working solution.
Contents of GB 31604.50-2020
1 Scope
2 Principle
3 Reagents and materials
4 Apparatus
5 Analysis steps
6 Expression of analysis results
7 Precision
8 Others
Annex A Reference mass spectrometry conditions
Annex B MRM chromatogram of nonylphenol standard working solution
