GB 5009.271-2016_English: PDF (GB5009.271-2016)
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Determination of phthalate esters in foods
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GB 5009.271-2016
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| Standard ID | GB 5009.271-2016 (GB5009.271-2016) | | Description (Translated English) | Determination of phthalate esters in foods | | Sector / Industry | National Standard | | Classification of Chinese Standard | X04 | | Classification of International Standard | 67.040 | | Word Count Estimation | 15,197 | | Date of Issue | 2016-12-23 | | Date of Implementation | 2017-06-23 | | Older Standard (superseded by this standard) | GB/T 21911-2008; SN/T 3147-2012 | | Regulation (derived from) | National Health and Family Planning Commission Notice No.17 of 2016 | | Issuing agency(ies) | National Health and Family Planning Commission of the People Republic of China, State Administration of Food and Drug Administration | | Summary | This standard specifies the method for the determination of 16 phthalate esters in food by gas chromatography-mass spectrometry (GC-MS). The second method specifies the content of 18 phthalate esters in food Determination of Gas Chromatography - Mass Spectrometry (GC - MS). The first method of this standard applies to food dimethyl phthalate (DMP), diethyl phthalate (DEP), diisobutyl phthalate (DIBP), di Ester (DBP), bis (2-methoxy) ethyl phthalate (DMEP), bis (4-methyl-2-pentyl) phthalate (BMPP), phthalic acid bis 2-ethoxy) ethyl ester (DEEP), dipentyl phthalate (DPP), phthalic acid di |
GB 5009.271-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Determination of phthalates in food
ISSUED ON. DECEMBER 23, 2016
IMPLEMENTED ON. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of PRC;
Food and Drug Administration.
Table of Contents
Foreword ... 4
1 Scope ... 5
2 Principle ... 5
3 Reagents and materials ... 6
4 Instruments and equipment... 7
5 Analytical procedures ... 8
6 Expression of analysis results ... 11
7 Precision ... 12
8 Other ... 12
9 Principle ... 12
10 Reagents and materials ... 12
11 Instruments and equipment ... 13
12 Analytical procedures ... 13
13 Expression of analysis results ... 15
14 Precision ... 15
15 Other ... 15
Appendix A Common phthalate plasticizer information sheet ... 16
Appendix B Monitoring ionic parameters of phthalates in isotope internal
standard method ... 17
Appendix C Total ion chromatogram of phthalate standard solution (isotope
internal standard method) ... 19
Appendix D Phthalate monitoring ionic parameters in external standard method
... 20
Appendix E Total ion chromatogram of phthalate standard solution (external
standard method) ... 21
Foreword
This standard replaces GB/T 21911-2008 “Determination of phthalate esters in
foods” and SN/T 3147-2012 “Determination of phthalates in exported foods”.
As compared with GB/T 21911-2008, the main changes of this standard are as
follows.
- CHANGE the standard name to “National food safety standard -
Determination of phthalates in food”;
- ADD two target compounds. diallyl phthalate and diisononyl phthalate;
- ADD the isotope internal standard method for quantification as the method
I;
- MODIFY the pre-processing method;
- MODIFY the method detection limit.
National food safety standard -
Determination of phthalates in food
1 Scope
The first method of this standard specifies the method for the determination of
the contents of 16 phthalate esters in food by gas chromatography-mass
spectrometry (GC-MS); the second method specifies the method for the
determination of the contents of 18 phthalates in foods gas chromatography-
mass spectrometry (GC-MS).
The first method of this standard applies to the determination and confirmation,
by the internal standard method, of the contents of Dimethyl phthalate (DMP),
Diethyl phthalate (DEP), Diisobutyl phthalate (DIBP), Dibutyl phthalate (DBP),
Bis (2-methoxyethyl) phthalate (DMEP), Bis(4-methyl-2-pentyl) phthalate
(BMPP), Bis(2-ethoxyethyl) phthalate (DEEP), Dipentyl phthalate (DPP),
Dihexyl phthalate (DHXP), Benzylbutyl phthalate (BBP), Bis (2-n-butoxyethyl)
phthalate (DBEP), Dicyclohexyl phthalate (DCHP), Bis (2-ethylhexyl) phthalate
(DEHP), Diphenylphthalate (DPhP), Di-n-octylphthalate (DNOP) and Dinonyl
phthalate (DNP) in foods; the second method is applicable to the determination
and confirmation, by the external standard method, of the contents of Dimethyl
phthalate (DMP), Diethyl phthalate (DEP), Diallyl phthalate (DAP), Diisobutyl
phthalate (DIBP), Dibutyl phthalate (DBP), Bis (2-methoxyethyl) phthalate
(DMEP), Bis(4-methyl-2-pentyl) phthalate (BMPP), Bis(2-ethoxyethyl)
phthalate (DEEP), Dipentyl phthalate (DPP), Dihexyl phthalate (DHXP),
Benzylbutyl phthalate (BBP), Bis (2-n-butoxyethyl) phthalate (DBEP),
Dicyclohexyl phthalate (DCHP), Bis (2-ethylhexyl) phthalate (DEHP),
Diphenylphthalate (DPhP), Di-n-octylphthalate (DNOP), Diisononyl ortho-
phthalate (DINP), Dinonyl phthalate (DNP) in foods.
Method I -- Gas chromatography - Mass spectrometry
- Isotope internal standard method
2 Principle
The deuterated phthalate is added to the specimen as an internal standard,
various foods are extracted and purified, and then determined by gas
chromatography-mass spectrometry. The characteristic selective ion
monitoring scan mode (SIM) is used, the ratio of the retention time to the
abundance of the qualitative ion fragments is used for qualitative, the isotope
internal standard method is used for quantification.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are
chromatographically pure, the water is the grade II water as specified in GB/T
6682.
3.1 Reagents
3.1.1 n-Hexane (C6H14).
3.1.2 Acetonitrile (C2H3N).
3.1.3 Acetone (CH3COCH3).
3.1.4 Dichloromethane (CH2Cl2).
3.2 Standard substance
3.2.1 The 16 phthalate standard substances
The mixed liquid standard substance of Dimethyl phthalate (DMP), Diethyl
phthalate (DEP), Diisobutyl phthalate (DIBP), Dibutyl phthalate (DBP), Bis (2-
methoxyethyl) phthalate (DMEP), Bis(4-methyl-2-pentyl) phthalate (BMPP),
Bis(2-ethoxyethyl) phthalate (DEEP), Dipentyl phthalate (DPP), Dihexyl
phthalate (DHXP), Benzylbutyl phthalate (BBP), Bis (2-n-butoxyethyl) phthalate
(DBEP), Dicyclohexyl phthalate (DCHP), Bis (2-ethylhexyl) phthalate (DEHP),
Di-n-octylphthalate (DNOP) and Dinonyl phthalate (DNP), Diphenylphthalate
(DPhP), the concentration is 1000 μg/mL, the standard substance information
and purity are as shown in Appendix A.
3.2.2 Phthalate internal standard substance of 16 deuterated isotopes
D4-Dimethyl phthalate (D4-DMP), D4-Diethyl phthalate (D4-DEP), D4-Diisobutyl
phthalate (D4-DIBP), D4-Dibutyl phthalate (D4-DBP), D4-Bis (2-methoxyethyl)
phthalate (D4-DMEP), D4-Bis(4-methyl-2-pentyl) phthalate (D4-BMPP), D4-
Bis(2-ethoxyethyl) phthalate (D4-DEEP), D4-Dipentyl phthalate (D4-DPP), D4-
Dihexyl phthalate (D4-DHXP), D4-Benzylbutyl phthalate (D4-BBP), D4-Bis (2-n-
butoxyethyl) phthalate (D4-DBEP), D4-Dicyclohexyl phthalate (D4-DCHP), D4-
Bis (2-ethylhexyl) phthalate (D4-DEHP), D4-Diphenylphthalate (D4-DPhP), D4-
Di-n-octylphthalate (D4-DNOP) and D4-Dinonyl phthalate (D4-DNP). purity >
99%.
3.3 Standard solution preparation
3.3.1 The 16 phthalate standard intermediate solutions (10 μg/mL). accurately
PIPETTE 1 mL of phthalate standard substance (1000 μg/mL) into a 100 mL
volumetric flask, USE the n-hexane to make its volume reach to the mark.
3.3.2 Phthalate internal standard solution of 16 deuterated isotopes (100
μg/mL). Accurately WEIGH 0.01 g of phthalate internal standard of 16
deuterated isotopes (accurate to 0.0001 g) into a 100 mL volumetric flask, USE
the n-hexane to make its volume reach to the mark.
3.3.3 Standard use solution of phthalate internal standard of 16 deuterated
isotopes (10 μg/mL). Accurately PIPETTE 10 mL of the phthalate internal
standard (100 μg/mL) of 16 deuterated isotopes in a 100 mL volumetric flask,
ADD n-hexane to make its volume reach to the mark.
3.3.4 The 16 phthalate standard series working solutions. Accurately TAKE 16
kinds of phthalate standard intermediate solution (10 μg/mL), USE n-hexane to
gradually dilute it to prepare the standard series solution of concentration 0.00
μg/mL. 0.02 μg/mL, 0.05 μg/mL, 0.10 μg/mL, 0.20 μg/mL, 0.50 μg/mL, 1.00
μg/mL, meanwhile ADD the internal standard use solution (10 μg/mL) to make
the concentration of the internal standard of 0.125 μg/mL, PREPARE it before
use.
4 Instruments and equipment
Note. After washing the glassware, it is rinsed 3 times with distilled water, it is
soaked in acetone for 1 hour, baked at 200 °C for 2 hours, and cooled to room
temperature to prepare for use.
4.1 Gas chromatography-Mass spectrometry (GC-MS).
4.2 Analytical balance. Accuracy 0.0001 g.
4.3 Nitrogen blowing instrument.
4.4 Vortex oscillator.
4.5 Ultrasonic generator.
4.6 Centrifuge. Speed ≥ 4000 r/min.
4.7 Crusher.
4.8 Solid phase extraction (SPE) device.
4.9 Solid phase extraction column. PSA/Silica composite packed glass column
(1000 mg, 6 mL).
5.2.2.2 Semi-solid specimen B. sesame sauce, oily sauce, etc.
After the sample is fully pulverized and mixed, accurately WEIGH 0.5 g
(accurate to 0.0001 g) into a 10 mL stoppered centrifuge tube, ADD 25 μL of
isotope internal standard solution, ADD 1 mL of n-hexane, VORTEX it for 2 min,
then ADD 5 mL of acetonitrile, VORTEX it for 1 min, PERFORM ultrasonic
extraction for 20 min, CENTRIFUGE at 4000 r/min for 5 min, COLLECT the
supernatant. ADD 5 mL of acetonitrile, PERFORM extraction again, COMBINE
the supernatant. USE 40 °C nitrogen to blow it dry, ADD 6 mL of acetonitrile,
VORTEX it uniformly to prepare for SPE purification.
5.2.3 Solid specimen
5.2.3.1 Solid specimen A. milk powder, rice flour, chicken essence,
monosodium glutamate, cheese, candy, pollen, meat products, cakes, instant
noodles, fruits and vegetables and their products, etc.
Accurately WEIGH 0.5 g (accurate to 0.0001 g) into a 25 mL stoppered
centrifuge tube, ADD 125 μL of isotope internal standard solution, ADD 2 mL ~
5 mL of distilled water, VORTEX it uniformly, then accurately ADD 10 mL of n-
hexane, VORTEX it for 1 min, vigorously SHAKE it for 1 min, PERFORM
ultrasonic extraction for 30 min, CENTRIFUGE it at 1000 r/min for 5 min, TAKE
the supernatant to prepare for GC-MS analysis.
5.2.3.2 Solid specimen B. butter, etc.
After the sample is fully pulverized and mixed, accurately WEIGH 0.5 g
(accurate to 0.0001 g) into a 10 mL stoppered centrifuge tube, ADD 25 μL of
isotope internal standard solution, ADD 1 mL of n-hexane, VORTEX it for 2 min,
then ADD 5 mL of acetonitrile, VORTEX it for 1 min, PERFORM ultrasonic
extraction for 20 min, CENTRIFUGE it at 4000 r/min for 5 min, COLLECT the
supernatant. ADD 5 mL of acetonitrile to make extraction again, COMBINE the
supernatant. USE 40 °C nitrogen to blow it almost dry, ADD 6 mL of acetonitrile,
VORTEX it uniformly to prepare for SPE purification.
Note. The butter shall be melted into liquid oil and mixed uniformly before being
weighed, it shall be kept in a liquid state during the extraction process.
5.3 SPE purification
ADD 5 mL of dichloromethane and 5 mL of acetonitrile for activation, DISCARD
the effluent; ADD the liquid to be purified to the SPE column, COLLECT the
effluent; then ADD 5 mL of acetonitrile, COLLECT the effluent, COMBINE the
two collected effluent, ADD 1mL of acetone, USE 40 °C nitrogen to blow it
almost dry, USE the n-hexane to make its volume reach to 2 mL, VORTEX it
uniformly to prepare for GC-MS analysis.
from the standard working curve, in micrograms per milliliter (μg/mL);
V - Constant volume of specimen, in milliliters (mL);
m - The mass of the specimen, in grams (g);
1000 - Conversion factor.
The calculation result shall be deducted from the blank value. When the result
is greater than or equal to 1.0 mg/kg, three significant figures are retained; when
the result is less than 1.0 mg/kg, two significant figures are retained.
7 Precision
The absolute difference between two independent determinations obtained
under repeatability conditions shall not exceed 10% of the arithmetic mean.
8 Other
The limit of quantification of the method is. the limit of quantification of di-n-butyl
phthalate (DBP) is 0.3 mg/kg, the limit of quantification of other 15 phthalates
except DBP is 0.5 mg/kg.
Method II -- Gas chromatography-mass spectrometry -
External standard method
9 Principle
Various foods are extracted and purified and determined by gas
chromatography-mass spectrometry. The characteristic selective ion
monitoring scan mode (SIM) is used, the retention time and qualitative ion
fragment abundance ratio are used for qualitative, the external standard
method is used for quantification.
10 Reagents and materials
Unless otherwise stated, the reagents used in this method are
chromatographically pure, the water is grade II water specified in GB/T6682.
10.1 Reagents
Same as 3.1.
Same as 5.1.
12.2 Specimen processing
Except that the isotope internal standard is not added, it is carried out in
accordance with the 5.2 determination procedure.
12.3 SPE purification
Same as 5.3.
12.4 Blank test
Except that no specimen is added, the measurement steps are carried out in
accordance with 12.2 and 12.3.
12.5 Instrument reference conditions
Except for the scanning method, the rest is same as 5.5.
Scanning method. Selective ion scan (SIM) and monitoring ions are as shown
in Appendix D.
12.6 Production of standard curve
Respectively INJECT the standard series working solution into the gas
chromatography-mass spectrometer, DETERMINE the chromatographic peak
area of the corresponding phthalate, USE the mass concentration of the
standard working solution as the abscissa and the corresponding peak area as
the ordinate, DRAW a standard curve. The Diisononyl ortho-phthalate standard
series working solution are injected for determination separately.
12.7 Determination of specimen solution
The sample solution was injected into a gas chromatography-mass
spectrometer to obtain a peak area of the corresponding phthalate, and the
concentration of the phthalate in the liquid to be tested was obtained in
accordance with a standard curve.
12.8 Qualitative confirmation
Under the conditions of 12.5 instrument, the target compound of the specimen
test solution and the phthalate standard appear at the same retention time
(±0.5%), and the mass-to-charge ratio of the mass spectrometry fragment ions
is consistent with the mass spectrum of the standard, which can be used to
qualify the target compounds.
See Appendix E for the total ion chromatogram of phthalates.
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