Search Result of Chinese Standard: 'GB 31604.28-2016'
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National Food Safety Standard - Food contact materials and products - Determination of di (2-ethylhexyl) adipate and migration
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GB 31604.28-2016
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Detail Information of GB 31604.28-2016; GB31604.28-2016
Description (Translated English): Method for the determination of di (2-ethylhexyl) adipatemigrating from polyvinyl chloride film in contact with foodstuffs
Sector / Industry: National Standard
Classification of Chinese Standard: X09
Word Count Estimation: 10,132
Date of Issue: 2016-10-19
Date of Implementation: 2017-04-19
Older Standard (superseded by this standard): SN/T 2826-2011 Partially; GB/T 20500-2006 Partially; GB/T 20499-2006
Regulation (derived from): State Health and Family Planning Commission Notice No.1516 of 2016
GB 31604.28-2016
Method for the determination of di (2-ethylhexyl) adipatemigrating from polyvinyl chloride film in contact with foodstuffs
National Standards of People's Republic of China
National food safety standards
Food contact materials and products adipic acid II
Determination of (2-ethyl)hexyl ester and determination of migration amount
Published on.2016-10-19
2017-04-19 Implementation
China
National Health and Family Planning Commission released
Foreword
This standard replaces GB/T 20499-2006 "Determination of migration of di-2-ethylhexyl adipate in polyvinyl chloride film for food packaging",
GB/T 20500-2006 "Determination of content of di(2-ethylhexyl) adipate and di-n-octyl adipate in polyvinyl chloride film"
Method for the determination of (2-ethylhexyl) ester content" and SN/T 2826-2011 "Food contact materials, polymeric materials, food analogs, adipic acid
Determination of Esters Plasticizers Gas Chromatography-Mass Spectrometry, Method for Determination of Migration of Di-2-ethylhexyl Adipate.
Compared with GB/T 20499-2006 and GB/T 20500-2006, the main changes are as follows.
---The standard name was changed to "National Food Safety Standard Food Contact Materials and Products Determination of Di-2-ethylhexyl Adipate
And determination of migration volume;"
--- Removed "Gas Chromatographic Method for Measuring Di(2-Ethylhexyl Adipate)".
National food safety standards
Food contact materials and products adipic acid II
Determination of (2-ethyl)hexyl ester and determination of migration amount
1 Scope
This standard specifies the determination method and migration of di-2-ethylhexyl adipate (DEHA) in food contact materials and products.
method.
This standard applies to the determination of di-2-ethylhexyl adipate in polyvinyl chloride products and the determination of migration.
Determination of di(2-ethylhexyl) adipate
2 principle
Tetrahydrofuran was used to dissolve the sample, and the polymer was precipitated by adding methanol. After filtration, DEHA was left in the filtrate and gas chromatography was used.
Spectrograph determination, external standard method.
3 Reagents and materials
3.1 Reagents
Unless otherwise stated, the reagents used in this method are of analytical grade, and the water is a grade one water according to GB/T 6682.
3.1.1 Tetrahydrofuran (C4H8O, CAS number. 109-99-9).
3.1.2 Methanol (CH4O, CAS number. 67-56-1).
3.1.3 n-hexane (C6H12, CAS number. 110-54-3). chromatographic purity.
3.2 Standards
Di(2-ethylhexyl) adipate (C22H42O4, CAS No.. 103-23-1). Purity ≥99.8%, or nationally certified and awarded to standards
The quality standard material.
3.3 standard solution preparation
3.3.1 DEHA standard stock solution
Weigh DEHA 100mg (accurate to 0.0001g), dissolved in n-hexane, to volume to 50mL, DEHA concentration was obtained
2mg/mL standard stock solution. The solution is stored in the refrigerator and is valid for 1 month.
3.3.2 DEHA standard intermediate solution
Use a graduated pipette to draw 2.5 mL of DEHA standard stock solution (3.3.1) into a 50 mL volumetric flask and dilute with n-hexane.
Degree, DEHA standard intermediate solution was obtained at a concentration of 100.0 mg/L. The solution is stored in the same manner as in 3.3.1.
3.3.3 DEHA standard working solution
Retrieval of 50 μL, 0.2 mL, 0.5 mL, 1.0 mL, 2.0 mL, and 5.0 mL of DEHA using a graduated pipette and a microsyringe, respectively
The standard intermediate solution (3.3.2) was placed in six 10 mL volumetric flasks, diluted with n-hexane, and the volume was fully shaken to obtain the concentrations as
0.5 mg/L, 2.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 50.0 mg/L DEHA standard working solution. Solution storage
Save the same with 3.3.1.
4 Instruments and Equipment
4.1 Gas Chromatography-Mass Spectrometer. Electron Impact Ion Source (EI).
4.2 Analytical balance (accuracy 0.1 mg).
4.3 Ultrasonic cleaners.
4.4 nitrogen blowing instrument.
4.5 Microsyringe. 100 μL.
4.6 test tube. 50mL.
Note. The glassware used in the experiment has been washed with methanol, ventilated and then used.
5 Analysis steps
5.1 sample processing
Take a sample, cut into 0.5cm x 0.5cm pieces with scissors and mix well.
5.2 Preparation of sample solution
Weigh 0.1g (accurate to 0.0001g) sample in 50mL test tube, add 5mL tetrahydrofuran, ultrasonic extraction 30min, to be sample
After all were dissolved, 25 mL of methanol was slowly added to precipitate the polyvinyl chloride polymer. The filter paper was filtered and washed three times with 5 mL of methanol.
The filtrates were combined in a 50 mL volumetric flask, brought to volume with methanol and mixed well, and 100 μL of the filtrate was blown dry with nitrogen at room temperature and brought to volume with n-hexane.
To 1.0 mL, to be tested. If the concentration of the sample exceeds the linear range of the standard working solution, it may be measured after proper dilution with n-hexane.
5.3 Preparation of Blank Solutions
Except without the sample, use the same analysis procedure, reagent and dosage as in 5.2.
5.4 Instrument Reference Conditions
5.4.1 chromatographic conditions
The chromatographic conditions are listed below.
a) Column. The stationary phase is (5%) diphenyl-(95%) dimethylarylene siloxane copolymer, column length 30m, inner diameter 0.32mm,
Film thickness 0.25μm;
b) column temperature program. the initial temperature is 90 °C, and then to 15 °C/min rate to 280 °C, hold 10min;
c) Inlet temperature. 280°C;
d) Carrier gas. helium 1.5mL/min;
e) sampling mode. diversion mode, split ratio is 50.1;
f) Injection volume. 0.2 μL.
5.4.2 Mass Spectrometry Conditions
The mass spectrometry conditions are listed below.
a) Mass spectrometry interface temperature. 250°C;
b) Ion source temperature. 250°C;
c) Ionization method. EI;
d) Ionization energy. 70 eV;
e) Measurement method. Select ion monitoring mode, DEHA monitoring ion range (m/z). 40~370, the characteristic ion of DEHA is
129, 147, 112, 71, where 129 is a quantitative ion;
f) Solvent delay. 5 min.
5.5 Draw a standard working curve
According to the measurement conditions listed in 5.4, the standard working solution (3.3.3) was injected into the gas chromatograph-mass spectrometer one by one, and the standard working solution was dissolved.
The concentration in the liquid is the abscissa, and the unit is milligrams per liter (mg/L). The standard curve is plotted with the DEHA peak area as the ordinate. standard color
See Figure A.1 for the spectrum.
5.6 Determination of sample solution
5.6.1 Qualitative determination
According to the measurement conditions listed in 5.4, the sample solution (5.2) and blank solution (5.3) were injected into a gas chromatograph-mass spectrometer. In the same real
When determining the sample under test conditions, if the retention time of the chromatographic peak of the analyte in the sample solution and the retention time of the corresponding standard chromatographic peak
The deviation is within ±2.5%, and in the subtracted background mass spectrum of the sample, all the selected ions appear, and the qualitative ions in the sample spectrum
The relative abundances of these compounds are compared with the relative abundances of the corresponding qualifier ions in the standard solution spectra close to the concentration, and the deviation does not exceed that specified in Table 1.
In the range, it can be determined that the sample is present in the sample. The characteristic ions of DEHA and their abundance ratio are shown in Table 2, and the DEHA mass spectrum is shown in Fig.2.
A.2.
Table 1 Maximum Allowable Deviation of Relative Ion Abundance in Qualitative Confirmation
Relative ion abundance K/% >50 20~50 10~20 ≤10
Allowable maximum deviation /% ±20 ±25 ±30 ±50
Table 2 Characteristic ions and abundance ratios of DEHA
Chemical Name Molecular Formula Qualitative Ion and Its Abundance Ratio Quantitative Ion
Di(2-ethylhexyl) adipate C22H42O4 129.12.1.47.71 = 100.25.25.31 129
5.6.2 Quantitative determination
When the sample and blank solution were measured, the blank value was subtracted to obtain the DEHA peak area.
6 Expression of analysis results
The DEHA content in the sample is calculated according to formula (1).
X=ρ×
V×f×10-6
m ×100%
(1)
In the formula.
X --- DEHA percentage content in the sample, %;
ρ --- DEHA concentration in the sample solution is determined from the working curve in milligrams per liter (mg/L);
V --- volume of solution in milliliters (mL);
f --- dilution factor;
10-6 --- unit conversion factor;
m --- The mass of the sample, in grams (g).
The calculation results retain two significant figures.
7 Precision
The absolute difference between two independent determinations obtained under repeatability conditions must not exceed 10% of its arithmetic mean.
8 Others
The detection limit of the method was 0.1% and the limit of quantification was 0.25%.
Determination of migration of di(2-ethylhexyl) hexanedioate
9 Principle
After the sample was soaked, di-2-ethylhexyl adipate migrated into the food simulant. After the liquid-liquid extraction, the extract was injected into the gas.
Detection by phase chromatography mass spectrometry, external standard method.
10 Reagents and Materials
Unless otherwise stated, the reagents used in this method are of analytical grade, and the water is a grade one water according to GB/T 6682.
10.1 Reagents
10.1.1 Water-based, acidic, alcoholic, oil-based food simulants. The reagents used are in accordance with the provisions of GB 31604.1.
10.1.2 n-Hexane (C6H14, CAS No. 110-54-3). Chromatographic purity.
10.1.3 Methanol (CH3OH, CAS Number. 67-56-1). Chromatographically pure.
10.1.4 Ethyl acetate (C4H8O2, CAS number. 141-78-6). Chromatographically pure.
10.2 reagent preparation
Water-based, acidic, alcoholic, oil-based food simulants. Operated according to GB 5009.156.
10.3 Standards
Di(2-ethylhexyl) adipate (DEHA, C22H42O4, CAS number. 103-23-1). Purity ≥99.8%, or certified by the country
And grant the standard substance certificate standard material.
10.4 Standard Solution Preparation
10.4.1 DEHA standard stock solution (for analysis of water-based, acidic, alcoholic food simulants)
Weigh 100 mg of DEHA standard (accurate to 0.0001 g), dissolve in n-hexane, and dilute to 50 mL to obtain DEHA concentration.
It is a standard stock solution of 2 mg/mL. The solution is stored in the refrigerator and is valid for 1 month.
10.4.2 DEHA standard intermediate solution (for analysis of water-based, acidic, and alcoholic food simulants)
Use a graduated pipette to draw 2.5 mL of DEHA standard stock solution (10.4.1) into a 50 mL volumetric flask and dilute to volume with n-hexane.
A DEHA standard intermediate solution was obtained with a concentration of 100.0 mg/L. The solution is stored in the same way as in 10.4.1.
10.4.3 DEHA standard working solution (for analysis of water-based, acidic, alcoholic food simulants)
Gradually pipette 50μL, 0.2mL, 0.5mL, 1.0mL, 2.0mL, 5.0mL DEHA with a graduated pipette and a micropipette.
The standard intermediate solution (10.4.2) was placed in six 10 mL volumetric flasks, diluted with n-hexane, and the volume was fully shaken to obtain the concentrations as
0.5 mg/L, 2.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 50.0 mg/L DEHA standard working solution. Solution storage
Save the same way as in 10.4.1.
10.4.4 DEHA standard stock solution (for analysis of oil-based food simulants)
Weigh DEHA 50mg (accurate to 0.0001g) into a 50mL beaker and add 50g of oil-based food simulant (accurate
0.0001g), dissolve and mix. The standard stock solution concentration is 1000mg/kg. The solution is stored in the refrigerator and is valid for 1 month.
10.4.5 DEHA standard intermediate solution (for analysis of oil-based food simulants)
Weigh 1.0g (accurate to 0.01g) DEHA standard stock solution (10.4.4) in a 10mL volumetric flask, and then weigh 9.0g accurately.
Indeed 0.0001g) oil-based food simulant was added to the volumetric flask and mixed to obtain DEHA standard intermediate solution at a concentration of
100mg/kg. The solution is stored in the same manner as in 10.4.4.
10.4.6 DEHA standard working solution (for analysis of oil-based food simulants)
Weigh 0.2g, 0.5g, 1.0g, 2.0g, 4.0g, 5.0g (accurate to 0.01g) DEHA standard intermediate solution (10.4.5) into
In six 10 mL volumetric flasks, add the oil-based food simulants 9.8g, 9.5g, 9.0g, 8.0g, 6.0g, and 5.0g (accurate
0.0001g), shake well, DEHA standard working solution. The solution concentrations were 2 mg/kg, 5 mg/kg, 10 mg/kg, 20 mg/kg, respectively.
40mg/kg, 50mg/kg. Accurately weigh 2.0g (accurate to 0.0001g) of the above solution into six 10mL centrifuge tubes.
Really add 2.0 mL of methanol, shake and extract for 10 min with a vortex shaker, stand for at least 30 min to separate the two phases and centrifuge them, and extract the upper layer.
The liquid was extracted by gas chromatography-mass spectrometry.
11 Instruments and Equipment
11.1 Gas Chromatography-Mass Spectrometer. Electron Impact Ion Source (EI).
11.2 nitrogen blowing instrument.
11.3 Centrifuge.
11.4 Vortex oscillator.
11.5 Centrifuge tube. 10 mL.
11.6 Constant temperature water bath.
Note. The glassware used in the experiment has been washed with methanol, ventilated and then used.
12 Analysis steps
12.1 Sample Migration Test
According to the requirements of GB 5009.156 and GB 31604.1, the samples were subjected to a migration test to obtain a food simulant test solution. If you get
The food simulant test solution cannot immediately proceed with the next test. The food simulant test solution should be stored in a refrigerator at 4°C in the dark.
The resulting food simulant test solution should be cooled or returned to room temperature before the next test.
12.2 Preparation of test solution
12.2.1 Preparation of Water-based, Acidic, Alcoholic Food Simulators
Use a graduated pipette to draw 2.0 mL mimic soak solution in a 10 mL centrifuge tube and accurately add 2.0 mL of B
The ethyl acid was extracted by shaking for 10 min, centrifuged at 4500 r/min for 5 min, and the ethyl acetate layer extract was removed; the solution was further extracted with 2.0 mL of ethyl acetate.
Take once, combine the two ethyl acetate extracts, dry with nitrogen at room temperature, and dilute to 2.0 mL with n-hexane for testing. If selected
If the content of ethanol in the food simulant exceeds 20%, the nitrogen gas blower is first used to remove the excess ethanol, and then the treatment is performed as described above.
12.2.2 Preparation of oil-based food simulants
Weigh 2.0g (accurate to 0.01g) of migration-tested oil-based food simulant soak solution in a 10mL centrifuge tube, accurately add
Into 2.0mL of methanol, shaking extraction with a vortex shaker for 10min, let stand for at least 30min to separate the two phases after centrifugation, sucking the upper extract
Gas chromatography-mass spectrometry analysis.
12.3 Preparation of Blank Solutions
The same analytical procedure, reagents and dosage as used in 12.2 were used except that no sample was added.
12.4 Instrument Reference Conditions
12.4.1 Gas chromatographic conditions
Gas chromatographic conditions are listed below.
a) Column. The stationary phase is (5%) diphenyl-(95%) dimethylarylene siloxane copolymer, column length 30m, internal diameter
0.32mm, film thickness 0.25μm;
b) column temperature program. the initial temperature is 90 °C, and then to 15 °C/min rate to 280 °C, hold 10min;
c) Inlet temperature. 280°C;
d) Carrier gas. nitrogen 1.5mL/min;
e) sampling mode. diversion mode, split ratio is 50.1;
f) Injection volume. 0.2 μL.
12.4.2 Mass Spectrometry Conditions
The mass spectrometry conditions are listed below.
a) Mass spectrometry interface temperature. 250°C;
b) Ion source temperature. 250°C;
c) Ionization method. EI;
d) Ionization energy. 70 eV;
e) Measurement method. Select ion monitoring mode, DEHA monitoring ion range (m/z). 40~370, the characteristic ion of DEHA is
129, 147, 112, 71, where 129 is a quantitative ion;
f) Solvent delay. 5 min.
12.5 Drawing Standard Operating Curves
According to the measurement conditions listed in 12.4, the standard working solution for water-based, acidic, alcoholic, oil-based food simulants (10.4.3,
10.4.6) Tests are performed with the DEHA concentration in the working soluti......
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