GB 31604.30-2016 (GB31604.30-2016)

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GB 31604.30-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard – Food Contact
Materials and Articles – Determination of the Content
and Migration of Phthalate Esters
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of PRC
Table of Contents
Foreword ... 4
1 Scope ... 5
2 Principle ... 5
3 Reagents and Materials ... 5
4 Apparatus ... 6
5 Analytical Procedures ... 7
6 Expression of Analytical Results ... 8
7 Precision ... 9
8 Others ... 9
9 Principle ... 9
10 Reagents and Materials ... 10
11 Apparatus ... 10
12 Analytical Procedures ... 11
13 Expression of Analytical Results ... 12
14 Precision ... 13
15 Others ... 13
Appendix A Information on 18 kinds of Commonly Used Phthalate Ester
Plasticizers ... 14
Appendix B Quantitative and Qualitative Selective Ion List of Phthalate Ester
Compounds ... 15
Appendix C Gas Chromatography – Mass Spectrometry Total Ion
Chromatogram of Phthalate Ester Standard Sample Solution ... 16
National Food Safety Standard – Food Contact
Materials and Articles – Determination of the Content
and Migration of Phthalate Esters
1 Scope
This Standard specifies the determination of the content and migration of phthalate
esters in the food contact materials and articles.
This Standard is applicable to the determination of the content of phthalate esters in
the food plastic packaging materials, and the determination of migration of phthalate
esters in food contact materials and articles.
Determination of Phthalate Esters
2 Principle
After crushing the food plastic packaging materials and articles, use n-hexane to
conduct the ultrasonic extraction; after filtering the extracting solution, use gas
chromatography-mass spectrometry to determine. Adopt the feature selective ion
monitoring scan mode (SIM), so that retain the qualitative of abundance ratio of the
time and fragments; use external standard method to quantify.
3 Reagents and Materials
Unless otherwise is specified, the reagents used in this Method are all
chromatographic pure (or analytically pure that has been redistilled). Water shall be
the one redistilled by a full glass device and stored in the glass vessel.
3.1 Reagents
3.1.1 N-hexane (C6H14).
3.12 Acetone (CH3COCH3).
3.2 Standard substance of phthalate esters
5 Analytical Procedures
5.1 Specimen preparation
Take 5g of typical sample; shear the specimen (excluding the preservative film) into
single pieces with diameter≤0.2cm; the preservative film piece diameter≤0.3cm; then
mix evenly; accurately take 0.2g~0.5g of specimen (accurate to 0.0001g) into
stoppered triangular flask; add 20mL of n-hexane; perform ultrasonic extraction for
30min and filter; after than the residue is re-extracted once by 20mL of n-hexane;
combine the filtrate into 50mL volumetric flask; use n-hexane to make constant volume
to the scale; then dilute it as per the content of phthalate esters in the specimen; after
mixing evenly, pass through a 0.45µm organic phase glass filter film; and be analyzed
in the gas chromatograph-mass spectrometer.
5.2 Blank test
The reagents used in the test shall be treated as per 5.1; and analyzed in GC-MS.
5.3 Instrument reference conditions
5.3.1 Gas chromatography reference conditions
a) Chromatographic column. 5% polyphenylmethylsiloxane quartz capillary column
or analytical column with similar performance; the specification indicates column
length of 30.0m, inner diameter of 0.25mm, film thickness of 0.25µm;
b) Sample inlet temperature. 260°C;
c) Temperature rise program. maintain the initial column temperature of 60°C for
1min; raise temperature to 220°C by 20°C/min, maintain for 1min; raise
temperature to 250°C by 5°C/min, maintain for 1min; then raise temperature to
290°C by 20°C/min, maintain for 7.5min;
d) Carrier gas. helium (purity >99.999%), flow rate. 1mL/min;
e) Sampling injecting method. splitless sample injection;
f) Sample injecting volume. 1µL.
5.3.2 Mass spectrometry reference conditions
a) Gas chromatography and mass spectrometry interface temperature. 280°C;
b) Ion source temperature. 230°C;
c) Ionization mode. electron impact ionization source (EI);
10 Reagents and Materials
Unless otherwise is specified, the reagents used in this Method are all
chromatographic pure (or analytically pure that has been redistilled). Water shall be
the one redistilled by a full glass device and stored in the glass vessel.
10.1 Reagents
10.1.1 N-hexane (C6H14).
10.1.2 Absolute alcohol (C2H5OH).
10.1.3 Acetic acid (CH3COOH).
10.1.4 Reagents required for preparing the acidic and alcoholic food simulants. abide
by the provisions of GB 31604.1.
10.1.5 Isooctane. oil-based food simulants.
10.2 Standard substance
The standard substance for 18 kinds of phthalate esters, the same as 3.2.
10.3 Preparation of standard solution
10.3.1 Standard stock solution. the same as 3.3.1.
10.3.2 17 kinds of phthalate esters standard use solutions. the same as 3.3.2.
10.3.3 Diisononyl ortho-phthalate standard use solution. the same as 3.3.3.
10.3.4 Phthalate ester standard serial working solution. accurately pipette
appropriate amount of phthalate ester standard use solution; use n-hexane to prepare
17 kinds of phthalate ester mixing standard use solutions with concentrations of
0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 3.0mg/L, 8.0mg/L, 10.0mg/L, as well as single-
labeled diisononyl ortho-phthalate (DINP) with concentrations of 0.5mg/L, 1.0mg/L,
3.0mg/L, 8.0mg/L, 10.0mg/L for later-use.
11 Apparatus
11.1 Gas chromatography-mass spectrometer. with electron impact source (EI).
11.2 Centrifuge.
11.3 Oscillator.
11.4 Solid phase extraction device.
11.5 Constant temperature oven.
11.6 Low-temperature incubator.
11.7 Centrifuge tube. 10mL.
11.8 Volumetric flask. 10mL.
11.9 Glassware.
NOTE. after washing the used glassware, rinse by the distilled water for 3 times; soak in
acetone for 1h; bake at 200°C for 2h; cool off to the room temperature for later-use.
12 Analytical Procedures
12.1 Preparation of food simulant test solution
According to the requirements of GB 5009.156 and GB 31604.1, perform the migration
test against the sample; then obtain the food simulant test solution.
12.2 Treatment of soaking solution
Place the soaking solution at the room temperature; for the isooctane and 95% ethanol
aqueous solution (≥ 50% alcoholic food) simulant soaking solution, accurately take
10g±0.01g of soaking solution into the pear-shaped distillation flask; reduce pressure
in 45°C water bath; perform rotary evaporation to dryness; add 1mL of n-hexane to
dissolve; perform vortex oscillation for 3min; centrifuge for 5min at 4000r/min; collect
the supernatant for the instrument test.
For other simulant soaking solutions (including water-based, acidic food, < 50%
alcoholic food simulant), take 10g±0.01g of simulant soaking solution into 25mL
centrifuge tube; add 4mL of n-hexane; shake and extract for 10min; centrifuge for 5min
at 4000r/min speed; take out the upper layer of n-hexane; repeatedly extract twice;
combine the n-hexane phase into pear-shaped distillation flask; reduce pressure in
45°C water bath; perform rotary evaporation to dryness; add 1mL of n-hexane to
dissolve; perform vortex oscillation for 3min; centrifuge for 5min at 4000r/min; collect
the supernatant for the instrument test.
The sample solution can be diluted as per the specific conditions, so that the measured
value shall be within the linear range of the standard curve.
12.3 Blank test
The reagents used in the test shall be treated as per 12.2; perform the GC-MS analysis.