GB 5009.

271-2016

National Food Safety Standard

Determination of Phthalate
Esters in Foods
食品安全国家标准
食品中邻苯二甲酸酯的测定

National Health and Family Planning

Commission of the People’s Republic of China
China Food and Drug Administration

Release Date: Dec 23, 2016

Implementation Date : Jun 23, 2017 Translated by ChemLinked
GB 5009.271-2016

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GB 5009.271-2016

National Standard of the People’s Republic of China

GB 5009.271-2016

National Food Safety Standard

Determination of Phthalate Esters in Foods
食品安全国家标准

食品中邻苯二甲酸酯的测定

Date of publication: 2016-12-23 Date of implementation: 2017-06-23

Issued by National Health and Family Planning Commission of the People’s Republic of China
China Food and Drug Administration

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GB 5009.271-2016

Foreword

This standard replaces GB/T 21911-2008 “Determination of phthalate esters in foods” and SN/T
3147-2012 “Determination of phthalate esters in food for export”.

Compared with GB/T 21911-2008, the main changes of this standard are as follows:

—the standard title has been revised to “National food safety standard Determination of phthalate
esters in foods”;

—two kinds of target compound including diallyl phthalate (DAP) and diisononyl ortho-phthalate
(DINP) have been added;

—the isotope internal standard quantitation has been added as the Method I;

—the pre-treatment method has been revised;

—the limit of detection for the method has been revised.

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GB 5009.271-2016

National Food Safety Standard

Determination of Phthalate Esters in Foods

1 Scope

Method I of this standard specifies the determination of 16 kinds of phthalate esters in foods by gas
chromatography-mass spectrometry (GC-MS); Method II specifies the determination of 18 kinds of
phthalate esters in foods by gas chromatography-mass spectrometry (GC-MS).

Method I of this standard applies to the internal standard determination and confirmation of the
content 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), benzyl
butyl phthalate (BBP), bis (2-n- butoxyethyl) phthalate (DBEP), dicyclohexyl phthalate (DCHP), bis
(2-ethylhexyl) phthalate (DEHP), diphenyl phthalate (DPhP), di-n-octyl phthalate (DNOP) and
dinonyl phthalate (DNP). Method II of this standard applies to the external standard determination
and confirmation of the content 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), benzyl butyl phthalate (BBP), bis (2-n-
butoxyethyl) phthalate (DBEP), dicyclohexyl phthalate (DCHP), bis (2-ethylhexyl) phthalate (DEHP),
diphenyl phthalate (DPhP), di-n-octyl phthalate (DNOP), diisononyl ortho- phthalate (DINP) and
dinonyl phthalate (DNP).

Method I Gas chromatography-mass spectrometry (GC-MS) Isotope internal standard

2 Principles

Deuterated phthalate esters were added to the test sample as the internal standard, and all kinds
of foods were extracted and purified, and then determined by the gas chromatography-mass
spectrometer. Using the characteristic selective ion monitoring (SIM) mode, qualitative analysis
was performed according to the retention time and the abundance ratio of qualitative ion segments
and quantitative analysis was performed by the isotope internal standard method.

3 Reagents and Materials

Unless otherwise specified, the reagents used in this method all refer to chromatographically pure

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GB 5009.271-2016

reagents and water used shall be Grade 2 water stipulated 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 substances

3.2.1 Standard substances of 16 kinds of phthalate esters

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), benzyl butyl
phthalate (BBP), bis (2-n-butoxyethyl) phthalate (DBEP), dicyclohexyl phthalate (DCHP), bis (2-
ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), dinonyl phthalate (DNP) and diphenyl
phthalate (DPhP), mixed liquid standard substances with the concentration of 1000μg/mL; see
Annex A for the information and purity of standard substances.

3.2.2 Internal standard of 16 kinds of deuterated isotopic phthalate esters

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-benzyl butyl phthalate (D4-BBP), D4-bis (2-n-
butoxyethyl) phthalate (D4-DBEP), D4-dicyclohexyl phthalate (D4-DCHP), D4-bis (2-ethylhexyl)
phthalate (D4-DEHP), D4-diphenyl phthalate (D4-DPhP), D4-di-n-octyl phthalate (D4-DNOP) and D4-
dinonyl phthalate (D4-DNP): with the purity of greater than 99%.

3.3 Preparation of standard solutions

3.3.1 16 kinds of phthalate esters standard intermediate solution (10μg/mL): accurately transfer
1mL of phthalate esters standard substances (1000μg/mL) to the 100-mL volumetric flask, and

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