GB 31604.29-2023 (GB31604.29-2023) & related versions
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National food safety standard - Food contact materials and products - Determination of migration of acrylic acid and methacrylic acid and their esters
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Food contact materials for export -- Polymers -- Determination of methyl methacrylate in food simulants -- Gas chromatography-mass spectrometry
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GB 31604.29-2023: PDF in English
GB 31604.29-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Food contact materials and
products - Determination of migration of acrylic acid and
methacrylic acid and their esters
ISSUED ON. SEPTEMBER 06, 2023
IMPLEMENTED ON. MARCH 06, 2024
Issued by. National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword... 3
1 Scope... 4
2 Principle... 4
3 Reagents and materials... 4
4 Instruments and apparatuses... 6
5 Analysis steps... 7
6 Expression of analysis results... 9
7 Precision... 11
8 Others... 11
9 Principle... 12
10 Reagents and materials... 12
11 Instruments and apparatuses... 14
12 Analysis steps... 14
13 Expression of analysis results... 15
14 Precision... 16
15 Others... 16
Appendix A Relevant information and weighing conversion coefficients of 18 acrylate
and methacrylate standards... 17
Appendix B Target retention time, quantitative ions and qualitative ions in gas
chromatography-tandem mass spectrometry SIM mode... 18
Appendix C Typical gas chromatography-tandem mass spectrometry total ion
chromatogram of standard working solution... 19
Appendix D Relevant information and weighing conversion coefficients of 6 acrylic
acid, methacrylic acid and their ester standards... 21
Appendix E Gradient elution reference procedure for liquid chromatography... 22
Appendix F Standard working solution liquid chromatogram... 23
National food safety standard -
Food contact materials and products - Determination of
migration of acrylic acid and methacrylic acid and their
esters
1 Scope
This Standard specifies the determination method for the migration of acrylic acid and
methacrylic acid and their esters in food contact materials and products.
Part 1 – Gas chromatography-mass spectrometry applies to the determination of
migration of 18 kinds of acrylate and methacrylate in food contact materials and
products, including 2-acrylic acid-2-methylpropyl ester, ethylacrylate, n-butyl acrylate,
isopropyl acrylate, acrylic acid n-propyl ester, 2-propenoic acid, 1,1-dimethylethyl ester,
acrylic acid benzyl ester, 2-octyl acrylate, sec-butyl acrylate, ethyl methacrylate,
isobutyl methacrylate, butyl methacrylate, 2-methyl-2-acrylic acid-1,1-dimethylethyl
ester, phenyl methacrylate, 2-methyl-2-propyl acrylate, benzyl methacrylate, sec-butyl
methacrylate and isopropyl methacrylate.
Part 2 – Liquid chromatography applies to the determination of migration of 6 kinds of
acrylic acid, methacrylic acid and their esters in food contact materials and products,
including acrylic acid, methacrylic acid, 2-hydroxyethyl acrylate, 2-hydroxyethyl-2-
methyl-2-acrylate, methyl acrylate and methyl methacrylate.
Part 1 – Gas chromatography-mass spectrometry
2 Principle
The water-based food simulants as well as oil and fat food simulants obtained from the
migration test are headspace sampled; the 95% (volume fraction) ethanol and isooctane
simulants are directly sample after diluted with ethyl acetate; the target substance is
separated in the gas chromatography capillary column, detected by mass spectrometry,
and quantified by the external standard method.
3 Reagents and materials
Unless otherwise specified, all the reagents in this method are analytical reagents, and
the water is grade-1 water specified by GB/T 6682.
3.1 Reagents
3.1.1 Methanol (CH4O). chromatographic pure.
3.1.2 Ethyl acetate (C4H8O2). chromatographic pure.
3.1.3 Sodium chloride (NaC1).
3.1.4 Anhydrous acetic acid (C2H4O2).
3.1.5 Absolute ethanol (C2H6O).
3.1.6 95% ethanol (C2H6O).
3.1.7 Isooctane (C8H18).
3.2 Preparation of reagents
3.2.1 Food simulant. Prepare in accordance with the provisions of GB 5009.156.
3.2.2 Isooctane-ethyl acetate solution (1+4). Mix 25 mL of isooctane and 100 mL of
ethyl acetate evenly.
3.2.3 95% ethanol-ethyl acetate solution (1+4). Mix 25 mL of 95% ethanol and 100 mL
of ethyl acetate evenly.
3.3 Standards
18 kinds of acrylate and methacrylate standards (see Appendix A). purity ≥98%, or
standard products certified by the country and awarded a standard substance certificate.
3.4 Preparation of standard solutions
3.4.1 Standard stock solutions (1 000 mg/L). Accurately weigh 18 standards (accurate
to 0.1 mg). The weighing mass calculation method is 25 mg divided by the conversion
coefficient, which is shown in Appendix A. Dissolve them in ethyl acetate respectively
and then transfer them to the 25 mL volumetric flasks; use ethyl acetate to dilute to the
mark and mix well. Transfer the solutions to brown glass containers and store them in
the dark at 4 °C for 6 months.
3.4.2 Mixture of standard intermediate solution A (50 mg/L). Respectively and
accurately pipette 0.5 mL of the standard stock solutions (1 000 mg/L) into the 10 mL
volumetric flasks; add methanol to adjust the volume to the mark; mix well. Transfer
the solutions to brown glass containers and store them in the dark at 4 °C for 6 months.
3.4.3 Mixture of standard intermediate solution B (50 mg/L). Respectively and
accurately pipette 0.5 mL of the standard stock solutions (1 000 mg/L) into the 10 mL
volumetric flasks; add ethyl acetate to adjust the volume to the mark; mix well. Transfer
the solutions to brown glass containers and store them in the dark at 4 °C for 6 months.
3.4.4 Water-based food simulant series standard working solutions. Respectively and
accurately pipette 100 μL, 150 μL, 200 μL, 400 μL and 1 000 μL of the mixtures of
standard intermediate solution A (50 mg/L) into the 100 mL volumetric flasks; use 50%
(volume fraction) ethanol solution to adjust the volume. The concentrations of each
target substance in the obtained standard working solutions are 0.050 mg/L, 0.075 mg/L,
0.10 mg/L, 0.20 mg/L, and 0.50 mg/L, respectively. Respectively pipette 10.0 mL of
solutions of each concentration into the 20 mL glass headspace bottles to which 3.0 g
of sodium chloride has been added; immediately use a spacer and an aluminum cap to
seal them, for later testing. Use the same method to prepare a series of standard working
solutions of the same concentration with water, 4% (volume fraction) acetic acid, 10%
(volume fraction) ethanol, and 20% (volume fraction) ethanol. Prepare when necessary.
3.4.5 Oil and fat food simulant series standard working solutions. Respectively and
accurately weigh 5.00 g (accurate to 0.01 g) of olive oil simulant into five 20 mL glass
headspace bottles; use a pipette to respectively pipette 30 μL, 80 μL, 100 μL, 150 μL,
and 300 μL of the mixture of standard intermediate solution B (50 mg/L) into the 20
mL glass headspace bottles; immediately use a spacer and an aluminum cap to seal them;
vortex evenly, for later testing. The concentrations of each target substance in the
obtained standard working solutions are 0.30 mg/kg, 0.80 mg/kg, 1.0 mg/kg, 1.5 mg/kg,
and 3.0 mg/kg, respectively. Prepare when necessary.
3.4.6 Isooctane series standard working solutions. Respectively pipette 50 μL, 150 μL,
200 μL, 300 μL and 600 μL of the mixture of standard intermediate solution B (50 mg/L)
into the 10 mL volumetric flasks; use isooctane-ethyl acetate solution (1+4) to adjust
the volume to the mark; mix well. The concentrations of each target substance in the
obtained standard working solution are 0.25 mg/L, 0.75 mg/L, 1.0 mg/L, 1.5 mg/L and
3.0 mg/L, respectively. Prepare when necessary.
3.4.7 95% (volume fraction) ethanol series standard working solutions. Respectively
pipette 50 μL, 150 μL, 200 μL, 300 μL, and 600 μL of the mixture of standard
intermediate solution B (50 mg/L) into the 10 mL volumetric flasks; use 95% ethanol-
ethyl acetate solution (1+4) to adjust the volume to the mark. The concentrations of
each target substance in the obtained standard working solution are 0.25 mg/L, 0.75
mg/L, 1.0 mg/L, 1.5 mg/L and 3.0 mg/L, respectively. Prepare when necessary.
4 Instruments and apparatuses
4.1 Gas chromatograph-mass spectrometer, equipped with electron impact source (EI)
and headspace sampler.
4.2 Vortex oscillator.
4.3 Electronic balance. The sensitivity is 0.1 mg and 0.01 g, respectively.
d) Oscillation speed. 500 r/min.
e) Injection volume. 250 μL.
5.4.2 The reference conditions for gas chromatography mass spectrometry
measurement are as follows.
a) Chromatographic column. polyethylene glycol capillary column. column length
30.0 m, inner diameter 0.25 mm, film thickness 0.25 μm, or an analytical column
with equivalent performance.
b) Programmed temperature rise. initial temperature 35 °C, kept for 8 min; increased
to 60 °C at 5 °C/min, kept for 3 min; increased to 160 °C at 20 °C/min, kept for
2 min; increased to 220 °C at 40 °C/min, kept for 3 min.
c) Inlet temperature. 290 °C.
d) Mass spectrometry joint temperature. 280 °C.
e) Ion source temperature. 230 °C;
f) Carrier gas. He (purity >99.999%), constant flow 1.0 mL/min.
g) Injection volume. 1 μL.
h) Injection method. split injection, the split ratio of water-based food simulant test
solution is 20.1; the split ratio of oil and fat food simulant test solution is 50.1;
the split ratio of isooctane test solution and 95% (volume fraction) ethanol test
solution is 2.1.
i) Ionization method. EI.
j) Solvent delay. 5.0 min.
k) Mass spectrometry scanning mode. selected ion mode (SIM).
l) SIM acquisition parameters. see Appendix B.
5.5 Preparation of the standard curve
According to the apparatus reference conditions listed in 5.4.1 and 5.4.2, inject the
series standard working solutions into the gas chromatograph-tandem mass
spectrometer respectively, and measure the corresponding peak areas. Draw the
standard working curve with the concentration of the target substance in the standard
series working solution as the abscissa and the corresponding quantitative ion peak area
as the ordinate. See Appendix C for the typical total ion chromatogram of standard
working solutions.
5.6 Qualitative determination
S – contact area between the sample and the soak solution in the migration test, in
square decimeters (dm2);
F – ratio (S/V) of the contact area (S) of food contact materials and products to the
volume (V) of food or food simulants under actual use conditions, in square
decimeters per kilogram (dm2/kg). In actual use situations, when S/V is known, F
is the actual S/V; when S/V cannot be estimated, F is 6 dm2/kg, that is, 6 dm2 of
food contact materials and products contact 1 kg of food or food simulants; the
density of various liquid foods is usually measured in 1 kg/L.
Express it as the arithmetic mean of two independent measurement results obtained
under repeatability conditions; retain 2 significant figures as the calculation result.
6.2 Calculation of specific migration of acrylic acid and methacrylic acid and their
esters in food contact materials and products such as sealed products (expressed
in mg/kg)
When the intended use is known, for food contact materials and products such as sealed
products, when the specific migration of acrylic acid, methacrylic acid and their esters
is expressed in mg/kg, it is calculated according to Formula (2).
Where.
X2 – specific migration of the target substance (based on acrylic acid/methacrylic acid),
in milligrams per kilogram (mg/kg);
c – content of the target substance (based on acrylic acid/methacrylic acid) in the sample
soak solution, in milligrams per liter (mg/L) or milligrams per kilogram (mg/kg);
c0 – content of the target substance (based on acrylic acid/methacrylic acid) in the blank
soak solution, in milligrams per liter (mg/L) or milligrams per kilogram (mg/kg);
V – volume or mass of the sample soak solution, in liters (L) or kilograms (kg);
S – contact area between the sample and the soak solution in the migration test, in
square decimeters (dm2);
S0 – area of the sealed product that comes into contact with food during actual use, in
square decimeters (dm2);
m2 – mass of solid food in the actual container used for sealed products, or mass of food
corresponding to the volume of actual contact with liquid food, in kilograms (kg);
the volume of various liquid foods is converted into the corresponding mass
according to the density of 1 kg/L.
of acrylic acid, methacrylic acid and their esters (based on acrylic acid and methacrylic
acid respectively) in oil and fat food simulants, isooctane and 95% (volume fraction)
ethanol are all 0.1 mg/kg, and the quantitation limits are 0.3 mg/kg. When the S/V in
the migration test is different from the S/V in actual use, this method converts the
detection limit and quantitation limit of the target substance in each food simulant and
chemical substitute solvent according to Chapter 6.
Part 2 – Liquid chromatography
9 Principle
The water-based food simulants and 95% (volume fraction) ethanol simulants obtained
from the migration test are filtered and directly injected. The oil and fat food simulants
and isooctane simulants are extracted with methanol and then injected. The target
substance is separated in a liquid chromatography column, detected with a UV detector
or diode array detector, and quantified using the external standard method.
10 Reagents and materials
Unless otherwise specified, all the reagents in this method are analytical reagents, and
the water is grade-1 water specified by GB/T 6682.
10.1 Reagents
10.1.1 Methanol (CH4O). chromatographic pure.
10.1.2 Acetonitrile (CH3CH). chromatographic pure.
10.1.3 Phosphoric acid (H3PO4). guaranteed reagent.
10.1.4 Anhydrous acetic acid (C2H4O2).
10.1.5 Absolute ethanol (C2H6O).
10.1.6 95% ethanol (C2H6O).
10.1.7 Isooctane (C8H18).
10.2 Preparation of reagents
10.2.1 Food simulant. Prepare in accordance with the provisions of GB 5009.156.
10.2.2 80% methanol solution. Measure 80 mL of methanol and 20 mL of water and
mix evenly.
10.2.3 0.1% phosphoric acid solution. Weigh 1.00 g of phosphoric acid into a 1 L
volumetric flask; use water to dilute to the mark; mix well.
10.3 Standards
6 kinds of standards of acrylic acid, methacrylic acid and their esters (see Appendix D).
purity ≥98%, or standard products certified by the country and awarded a reference
material certificate.
10.4 Preparation of standard solution
10.4.1 Standard stock solution (1 000 mg/L). Accurately weigh 6 standards (accurate to
0.1 mg). The weighing mass calculation method is 25 mg divided by the conversion
coefficient. The conversion coefficient is shown in Appendix D. Dissolve them in
methanol respectively and transfer them into the 25 mL volumetric flasks; use methanol
to dilute to the mark; mix well. Transfer the solutions to brown glass containers and
store them in the dark at 4 °C for 6 months.
10.4.2 Mixture of standard intermediate solution (50 mg/L). Respectively and
accurately pipette 0.5 mL of the standard stock solution (1 000 mg/L) into the 10 mL
volumetric flasks; add methanol to adjust the volume to the mark; mix well. Transfer
the solutions to brown glass containers and store them in the dark at 4 °C for 6 months.
10.4.3 Water-based food simulant series standard working solution. Respectively and
accurately pipette 25 μL, 50 μL, 100 μL, 200 μL, 500 μL of the mixture of standard
intermediate solution (50 mg/L) into the 5 mL volumetric flasks; use 50% (volume
fraction) ethanol solution to adjust the volume. The concentrations of each target
substance in the obtained standard working solution are 0.25 mg/L, 0.50 mg/L, 1.0
mg/L, 2.0 mg/L, and 5.0 mg/L, respectively. Use the same method to prepare standard
working solutions of the same concentration series with water, 4% (volume fraction)
acetic acid, 10% (volume fraction) ethanol, and 20% (volume fraction) ethanol. Prepare
when necessary.
10.4.4 Oil and fat food simulant series standard working solutions. Respectively weigh
5.00 g (accurate to 0.01 g) of olive oil simulant into 6 centrifuge tubes; use a pipette to
respectively pipette 30 μL, 60 μL, 100 μL, 150 μL and 300 μL of the mixture of standard
intermediate solutions (50 mg/L); vortex and mix; add 5 mL of methanol; vortex for 1
min; centrifuge at 4 000 r/min for 5 min; pass the upper solution through a microporous
filter membrane before testing. The concentrations of each target substance in the
obtained standard working solutions are 0.30 mg/kg, 0.60 mg/kg, 1.0 mg/kg, 1.5 mg/kg,
and 3.0 mg/kg, respectively. Prepare when necessary.
10.4.5 Isooctane series standard working solution. Respectively pipette 5.00 mL of
isooctane into 6 centrifuge tubes; use a pipette to respectively pipette 30 μL, 60 μL, 100
μL, 120 μL, 300 μL of the mixture of standard intermediate solution (50 mg/L); vortex
and mix; then, add 5.00 mL of 80% methanol solution; vortex and mix for 1 minute;
centrifuge at 4 000 r/min for 5 minutes; remove the lower solution and filter it before
testing. The concentrations of each target substance in the obtained standard working
12.3 Preparation of blank test solution
Follow the steps described in 12.1 and 12.2 to process food simulants, isooctane and
95% (volume fraction) ethanol simulants that are not in contact with food contact
materials.
12.4 Apparatus reference conditions
The reference conditions for liquid chromatography determination are as follows.
a) Chromatographic column. C18 column, column length 100 mm, inner diameter
4.6 mm, particle size 3 μm or analytical column of equivalent performance.
b) Mobile phase. 0.1% phosphoric acid solution (A) and acetonitrile (B). See
Appendix E for the gradient elution procedure.
c) Flow velocity. 1.0 mL/min.
d) Detection wavelength. 210 nm.
e) Injection volume. 20 μL;
f) Column temperature. 30 °C.
12.5 Drawing of the standard curve
According to the instrument reference conditions listed in 12.4.1, respectively inject the
series standard working solutions into the liquid chromatograph and measure the
corresponding peak areas. Draw the standard working curve with the concentration of
the target substance in the standard working solution as the abscissa and the
corresponding peak area of the target substance as the ordinate. See Appendix F for
typical liquid chromatograms of standard working solutions.
12.6 Determination of test solution
According to the instrument reference conditions listed in 12.4.1, inject the sample
solution (12.2) and blank test solution (12.3) sequentially to obtain the peak area of the
target substance. Calculate the concentrations c and c0 of the target substance in the
sample solution and blank test solution based on the standard curve.
13 Expression of analysis results
Same as Chapter 6.
......
| Standard ID | GB 31604.29-2023 (GB31604.29-2023) | | Description (Translated English) | (National Food Safety Standards Food Contact Materials and Products Determination of Multi-Elements and Determination of Multi-Element Migration Amounts) | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Word Count Estimation | 20,245 | | Date of Issue | 2023-09-06 | | Date of Implementation | 2024-03-06 | | Issuing agency(ies) | National Health Commission of the People's Republic of China, State Administration for Market Regulation | | Summary | This standard specifies the determination of arsenic, cadmium, chromium and lead in food contact materials and products and the determination of aluminum, arsenic, barium, cadmium, cobalt, chromium, copper, iron, lithium, manganese, molybdenum, nickel, lead, antimony, tin and Determination of zinc migration. The first article is applicable to the determination of arsenic, cadmium, chromium and lead in food contact paper and cardboard materials and products, cork stoppers and bamboo and wood products. Part II applies to plastic materials and products for food contact, paints and coatings for food contact, rubber materials and products for food contact, inks for food contact materials and products, adhesives for food contact materials and products, and paper for food contact Aluminum, arsenic, barium, cadmium, cobalt, chromium, copper, iron, lithium, manganese in cardboard materials and products, pacifiers, enamel products, ceramic products, glass products, food contact plastic resins, food contact metal materials and products , molybdenum, nickel |
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