Powered by Google-Search & Google-Books www.ChineseStandard.net Database: 169760 (Feb 27, 2021)
HOME   Quotation   Tax   Examples Standard-List   Contact-Us   View-Cart
  

GB 31604.50-2020

Chinese Standard: 'GB 31604.50-2020'
Standard IDContents [version]USDSTEP2[PDF] delivered inStandard Title (Description)StatusRelated Standard
GB 31604.50-2020English179 Add to Cart Days<=3 National food safety standard - Food contact materials and articles - Determination of nonylphenol migration Valid GB 31604.50-2020
GB 31604.50-2020Chinese17 Add to Cart <=1-day [PDF from Chinese Authority, or Standard Committee, or Publishing House]  

   

BASIC DATA
Standard ID GB 31604.50-2020 (GB31604.50-2020)
Description (Translated English) National food safety standard - Food contact materials and articles - Determination of nonylphenol migration
Sector / Industry National Standard
Word Count Estimation 9,942
Date of Issue 2020-09-11
Date of Implementation 2021-03-11
Regulation (derived from) National Health Commission Announcement No. 7 (2020) of the State Administration for Market Regulation

GB 31604.50-2020
National food safety standard-Food contact materials and articles-Determination of nonylphenol migration
National Standards of People's Republic of China
National Food Safety Standard
Food contact materials and products
Determination of migration of nonylphenol
2020-09-11 released
2021-03-11 implementation
National Health Commission of the People's Republic of China
Issued by the State Administration for Market Regulation
National Food Safety Standard
Food contact materials and products
Determination of migration of nonylphenol
1 Scope
This standard specifies the liquid chromatography-mass spectrometry/mass spectrometry method for the determination of nonylphenol migration of food contact materials and products.
This standard applies to food contact materials and products with water, 4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20%
(Volume fraction) ethanol solution, 50% (volume fraction) ethanol solution, olive oil, 95% (volume fraction) ethanol solution are food simulants or
Using 95% (volume fraction) ethanol solution and isooctane as a chemical substitute solvent to determine the nonylphenol in the soaking solution obtained by migration test.
2 Principle
Take 4% (volume fraction) acetic acid solution as the food simulant, the soaking solution obtained by migration test is added to ammonia water to neutralize the sample; take olive
The oil is a food simulant and the soaking liquid obtained from the migration test is sampled and determined after acetonitrile extraction and n-hexane purification; isooctane is used as a chemical substitute
After the soaking liquid obtained from the migration test is evaporated to dryness, it is reconstituted with methanol, and the sample is injected for determination; other soaking liquids and chemical substitute solvents obtained from the migration test are soaked
The liquid is directly injected for determination. The nonylphenol in the soaking solution was determined by liquid chromatography-mass spectrometry/mass spectrometry and quantified by external standard method.
3 Reagents and materials
Unless otherwise specified, the reagents used in this method are analytically pure, and the water is the first-grade water specified in GB/T 6682.
3.1 Reagents
3.1.1 Glacial acetic acid (C2H4O2).
3.1.2 Absolute ethanol (C2H6O).
3.1.3 95% ethanol.
3.1.4 Isooctane (C8H18).
3.1.5 Olive oil. chemically pure, in line with the requirements of 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. chromatographically pure, volume fraction ≥ 25%.
3.2 Reagent preparation
4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20% (volume fraction) ethanol solution, 50% (volume fraction) ethyl acetate
The preparation of alcohol solution is operated according to GB 5009.156.
3.3 Standard products
Nonylphenol (a mixture of branched chain isomers, C15H24O, CAS number. 84852-15-3) standard solution. 1000mg/L.
3.4 Preparation of standard solution
3.4.1 Standard Intermediate Solution (100mg/L)
Accurately pipette 1.00mL of nonylphenol standard solution (1000mg/L) into a 10mL volumetric flask, dilute with methanol and dilute to the mark.
Mix well. This solution is stored in a refrigerator at 0℃~4℃, and the validity period is 6 months.
3.4.2 Standard Intermediate Solution (5mg/L)
Accurately pipette 0.50 mL of nonylphenol standard intermediate solution (100 mg/L) into a 10 mL volumetric flask, dilute with methanol and dilute to the mark.
Mix well.
3.4.3 Standard working solution
3.4.3.1 4% (volume fraction) acetic acid standard working solution
Accurately pipette the standard intermediate solution (5mg/L) 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL, 0.40mL into 6
In a 10mL volumetric flask, dilute to the mark with 4% (volume fraction) acetic acid solution. The mass concentrations are 0.01mg/L, 0.02mg/L,
0.03mg/L, 0.05mg/L, 0.10mg/L, 0.20mg/L standard working solution. Before getting on the machine, follow 5.1.2.1 with food simulant soaking liquid
Synchronous processing.
3.4.3.2 Oil-based food simulant standard working solution
Accurately weigh 5.00g (accurate to 0.1mg) olive oil into 6 glass centrifuge tubes with stoppers, and add standard intermediate solution respectively
(5mg/L) 0.01mL, 0.02mL, 0.03mL, 0.05mL, 0.10mL, 0.20mL, vortex and mix to obtain 0.01mg/kg,
0.02mg/kg, 0.03mg/kg, 0.05mg/kg, 0.10mg/kg, 0.20mg/kg standard working solution. Follow 5.1.2.2 before boarding
Simultaneous processing with food simulant soaking liquid.
3.4.3.3 Isooctane standard working solution
Accurately pipette the standard intermediate solution (5mg/L) 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL, 0.40mL in
In 6 10mL volumetric flasks, make the volume up to the mark with isooctane, mix well, and obtain mass concentrations of 0.01mg/L, 0.02mg/L,
0.03mg/L, 0.05mg/L, 0.10mg/L, 0.20mg/L standard working solution. Before using the machine, it must be immersed with food simulant according to 5.1.2.3
Simultaneous treatment of bubble fluid.
3.4.3.4 Standard working solutions for other food simulants and chemical alternative solvents
Pipette standard intermediate solution (5mg/L) 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL, 0.40mL into 6 10mL
In the volumetric flask, use the corresponding food simulant or chemical substitute solvent to make the volume to the mark, and obtain the mass concentration of 0.01mg/L,
0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L, 0.20mg/L of other water-based food simulants or chemical substitute solvent standards
Quasi working solution.
4 Apparatus and equipment
4.1 Liquid chromatography tandem triple quadrupole mass spectrometer. distribution spray ion source (ESI).
4.2 Vortex oscillator.
4.3 Analytical balance. Sensitivity 0.0001g, 0.01g.
4.4 High-speed centrifuge. the highest speed>10000r/min.
5 Analysis steps
5.1 Preparation of test solution
5.1.1 Migration test
Food contact materials and products shall undergo migration test in accordance with the requirements of GB 31604.1 and GB 5009.156.Immersion from migration test
If the solution cannot be tested immediately, it should be stored in a refrigerator at 4℃ and protected from light. For the next test, the soaking solution should be restored to room temperature before use.
5.1.2 Treatment of soaking liquid
5.1.2.1 Treatment of 4% (volume fraction) acetic acid soaking solution
Pipette 5.0 mL of the 4% (volume fraction) acetic acid soaking solution obtained from the migration test, add 0.5 mL of ammonia and mix well, then pass 10000r/min
After centrifugation for 5 min, the supernatant was ready for testing.
5.1.2.2 Treatment of oil-based food simulants
Weigh 5.00g (accurate to 0.01g) of the olive oil soaking solution obtained from the migration test into a stoppered glass centrifuge tube, and add 2mL of n-hexane to mix
Then add 5.0mL acetonitrile, vortex for 0.5min, centrifuge at 4000r/min for 5min, take the upper layer of acetonitrile solution and separate at 10000r/min.
Heart for 5min, and the supernatant is to be tested.
5.1.2.3 Treatment of isooctane soaking solution
Pipette 10.0 mL of the isooctane soaking solution obtained from the migration test, rotate it to near dryness at 40°C, accurately pipette 10.0 mL of methanol to dissolve the residue,
After centrifugation at 10000r/min for 5min, the supernatant is ready to be tested.
5.1.2.4 Treatment of other food simulant soaking liquid and chemical substitute solvent soaking liquid
Pipette an appropriate amount of the soaking liquid obtained from the migration test, centrifuge at 10000r/min for 5min, and the supernatant is to be tested.
5.1.3 Preparation of blank test solution
According to 5.1.1 and 5.1.2, dispose of food simulants and chemical substitute solvents that are not in contact with food contact materials and products.
5.2 Instrument reference conditions
5.2.1 Liquid chromatography conditions
The reference conditions of liquid chromatography are as follows.
a) Chromatographic column. C18 column, 2.6μm, 2.1mm×150mm (or equivalent chromatographic column).
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 negative ion mode (ESI-).
b) Mass spectrometry scan mode. multiple reaction monitoring (MRM).
c) For other mass spectrometer parameters, see Table A.1 in Appendix A.
5.3 Drawing of standard curve
According to the instrument reference conditions listed in 5.2, the standard working solution is measured, and the concentration of nonylphenol in the standard working solution is used as the horizontal
The standard curve is drawn with the corresponding quantitative ion peak area as the ordinate, and the linear equation is obtained. Chromatogram of nonylphenol standard working solution
See Appendix B.
5.4 Determination of test solution
5.4.1 Qualitative determination
According to the instrument reference conditions listed in 5.2, determine the food simulant test solution and standard working solution. If the test solution and the standard solution are tested
The deviation of the retention time of the mass chromatographic peak is within ±2.5%; the signal-to-noise ratio of all qualifier ions exceeds 3.1, and the phase of the qualifier ion pair
The relative abundance of the standard solution with the same abundance and concentration is consistent, and the relative abundance deviation does not exceed the provisions of Table 1, then it can be judged that the sample exists
The corresponding DUT.
5.4.2 Quantitative determination
According to the instrument reference conditions listed in 5.2, the sample solution (5.1.2) and blank solution (5.1.3) are measured respectively to obtain the target peak
Area, calculate the nonylphenol content c and c0 in the sample solution and blank solution from the standard curve, and the nonylphenol content c0 in the blank solution should not be higher than
Method detection limit concentration.
6 Expression of analysis results
6.1 Calculation of the specific migration amount of nonylphenol for food contact materials and products of non-sealed products (expressed in mg/kg)
For food contact materials and products other than lids, sealing rings, connectors and other sealed products (hereinafter referred to as sealed products), Nonyl
When the specific migration amount of phenol is expressed in mg/kg, it is calculated according to formula (1).
The result retains at least 2 significant digits.
6.2 Calculation of specific migration amount of nonylphenol for food contact materials and products of sealed products (expressed in mg/piece)
When the intended use is unknown, when the specific migration amount of nonylphenol of sealed product-type food contact materials and products is expressed in mg/piece, according to formula (2)
For calculation, it is necessary to indicate the used migration test method and the contact area of a single sealed product with the food simulant in the migration test.
7 Precision
The absolute difference between two independent determination results obtained under repeatability conditions should not exceed 10% of its arithmetic mean.
8 other
When the S/V in the migration test is the same as the S/V in the actual use situation, this method is used for the nonyl in each food simulant and chemical substitute solvent.
The detection limit of phenol is 0.005mg/kg, and the limit of quantification is 0.01mg/kg.
Appendix A
Reference mass spectrometry conditions
The reference mass spectrometry conditions are as follows.
a) Curtain air. 69kPa.
b) Collision gas. 55kPa.
c) Spray voltage. -4500V.
d) Auxiliary gas temperature. 425℃.
e) Atomizing gas. 345kPa.
f) Auxiliary gas. 345kPa.
g) Other mass spectrometer parameters are shown in Table A.1.
Related standard: GB 31604.41-2016    GB 31604.30-2016