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GB 5009.271-2016 PDF English

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GB 5009.271-2016: National food safety standard - Determination of phthalates in food
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GB 5009.271-2016: National food safety standard - Determination of phthalates in food

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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). 3.2 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), 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).

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. 4.5 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 Analytical procedures

5.1 Specimen preparation 5.2 Specimen processing 5.2.1 Liquid specimen 5.2.1.1 Liquid specimen A. liquid milk, beverage, soy sauce, vinegar, liquor, honey, etc. 5.2.1.2 Liquid specimen B. vegetable oil, etc. MIX the liquid fat uniformly, accurately WEIGH 0.5 g (accurate to 0.0001 g) in a 10 mL centrifuge tube, ADD 25 μL of isotope internal standard solution, ADD 100 μL of n-hexane and 2 mL of acetonitrile in order, VORTEX it for 1 min, PERFORM ultrasonic extraction for 20 min, CENTRIFUGE it at 4000 r/min for 5 min, COLLECT the supernatant. 5.2.2 Semi-solid specimen 5.2.2.1 Semi-solid specimen A. jelly, sweet sauce, etc. Accurately WEIGH 0.5 g (accurate to 0.0001 g) of the uniformly mixed specimen in 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 Solid specimen 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. 5.4 Blank test Except that no specimen is added, the determination procedures are carried out in accordance with 5.2 and 5.3. Note. It shall avoid contact with plastic products throughout the operation. 5.5 Instrument reference conditions 5.5.1 Gas chromatography reference conditions 5.5.2 Mass spectrometry reference conditions 5.5.2.1 Ionization mode. electron bombardment ionization source (EI); 5.5.2.2 Ionization energy. 70 eV; 5.6 Production of standard curve Respectively INJECT the standard series working fluids into the gas chromatography-mass spectrometer, USE the peak area ratios of the phthalate components and their corresponding deuterated isotope internal standard as the ordinate, USE the ratio of the content of each component of the series standard solution (μg/mL) to the content of the corresponding deuterated isotope internal standard content (μg/mL) as the abscissa, to draw a standard curve. 5.7 Determination of specimen solution INJECT the specimen solution into a gas chromatography-mass spectrometer, USE the ratio of each component of the phthalate in the specimen to its internal standard peak area for quantitative calculation, to obtain the ratio of the content of each component in the specimen solution (μg/mL) to the corresponding internal isotope internal standard content (μg/mL). 5.8 Qualitative confirmation Under 5.5 instrument conditions, 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 corresponding mass spectrometry ion is consistent to the mass spectrum of the standard substance, the comparison of its abundance ratio with that of the standard substance shall comply with Table 1, which can be used to characterize the target compound.

6 Expression of analysis results

The content of phthalates in the specimen is calculated in accordance with formula (1).

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.

9 Principle

Various foods are extracted and purified and determined by gas chromatography-mass spectrometry. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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