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ICS 71.100.01; 87.060.10

G 55

National Standard of the People’s Republic of China

GB/T 37040-2018

Limit and determination of

carcinogenic dyes in dye products
染料产品中致癌染料的限量和测定

(English Translation)

Issue date: 2018-12-28 Implementation date: 2019-11-01

Issued by the State Administration for Market Regulation
the Standardization Administration of the People’s Republic
of China

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Contents

Foreword ............................................................................................................................... i
1 Scope ............................................................................................................................. 1
2 Normative references ..................................................................................................... 1
3 Requirements ................................................................................................................. 1
4 Theory ............................................................................................................................ 1
5 Test methods .................................................................................................................. 1
6 Minimum limit of detection, precision and recovery rate................................................ 6
7 Test report ...................................................................................................................... 6
Annex A Normative) Detection wavelength in HPLC-DAD method and characteristic ion
in HPLC-MS method of carcinogenic dyes .......................................................................... 8
Annex B (Informative) Schematic diagram for chromatogram of standard working
solution in HPLC/DAD method under detection wavelengths ............................................. 9

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Foreword

ChinaStandards.net is in charge of this English translation. In case of any doubt about

the English translation, the Chinese original shall be considered authoritative.

This standard is developed in accordance with the rules given in GB/T 1.1-2009.

This standard was proposed by the China Petroleum and Chemical Industry Association.

This standard is under the jurisdiction of SAC/TC 134 Technical Committee on Dyestuff of
Standardization Administration of China.

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Limit and determination of carcinogenic dyes in

dye products

Warning: the personnel using this standard shall have practical experience in
standard laboratory work. This standard does not purport to address all of the
safety problems, if any, associated with its use. It is the responsibility of the user to
establish appropriate safety and health practices and to ensure compliance with
any national regulatory conditions.

1 Scope

This standard specifies the limit and determination methods for 12 kinds of carcinogenic
dyes (see Annex A) in dye products.

This standard is applicable to dye products of each dosage form.

2 Normative references

The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.

GB/T 6682-2008 Water for analytical laboratory use - Specification and test methods (ISO
3696:1987, MOD)
GB/T 8170-2008 Rules of rounding off for numerical values & expression and judgement of
limiting values

3 Requirements

The content of all carcinogenic dyes (see Annex A) in dye products shall not be more than
150 mg/kg.

4 Theory

After the sample is dissolved (or extracted), carry out qualitative determination through
high-performance liquid chromatography-diode array detector (HPLC-DAD) method and
quantitative determination for carcinogenic dyes through peak area external standard
method; carry out qualitative determination for uncertain sample detected through liquid
chromatography-tandem mass spectrometry (HPLC-MS).

5 Test methods

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5.1 General requirements

Unless otherwise specified, only recognized analytically pure reagents and Grade-III
water (specified in GB/T 6682-2008) shall be adopted. The inspection result shall be
judged according to the rounding-off value comparison method specified in 4.3.3 of GB/T
8170-2008.

5.2 Reagents and materials

5.2.1 Standard carcinogenic dyes (see Annex A).

5.2.2 Methanol: chromatographically pure.

5.2.3 Acetonitrile, chromatographically pure.

5.2.4 n-tetrabutyl ammonium bromide.

5.2.5 Potassium dihydrogen phosphate.

5.2.6 Ammonium acetate.

5.3 Instruments and apparatus

5.3.1 Liquid chromatograph: infusion pump - with a flow rate range of 0.1 mL/min~5.0
mL/min, in which the flow stability is ± 1%; with a diode array detector.

5.3.2 Liquid chromatography-mass spectrometer: equipped with electrospray ionization.

5.3.3 Chromatographic working station or integrator.

5.3.4 Flat-head microinjector.

5.3.5 Ultrasonic generator.

5.3.6 Ground conical flask with stopper: 150 mL.

5.3.7 0.45μm polytetrafluoroethylene (PTFE) film filter head.

5.4 Preparation of standard solutions

5.4.1 Standard stock solution (200 mg/L)

Prepare a standard stock methanol solution of mono-component carcinogenic dye

standard sample as listed in Annex A, with an effective concentration of 200 mg/L, store in

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the freezer in a refrigerator free of light, with a validity period of 1 year.

5.4.2 Standard working solution

Group A: pipette 0.5 mL of Basic violet 14 standard stock solution into a 50-mL volumetric
flask and dilute it with methanol to the scale.

Group B: pipette 0.5 mL of solutions from the rest 11 standard stock solutions into 50-mL
volumetric flasks respectively and dilute them with methanol to the scale.

The standard working solution may be prepared immediately before use to be those with
other suitable concentrations as required.

5.5 Preparation of sample solution

Methanol-soluble dye: weigh 0.5 g of specimen (accurate to 0.0001 g), place it in a 50-mL
volumetric flask, dissolve it with methanol, dilute it to the scale, vibrate and fully dissolve it
in an ultrasonic generator for standby.

Methanol-insoluble dye: weigh 0.5 g of specimen (accurate to 0.0001 g), place it in a

100-mL ground conical flask with a stopper, add 50 mL of methanol accurately, extract it in
an ultrasonic generator for 30 min, cool it to room temperature, and filter the extract with a
0.45 μm polytetrafluoroethylene film filter head for standby.

5.6 Chromatographic analysis

5.6.1 HPLC-DAD analysis method

5.6.1.1 HPLC-DAD chromatographic conditions

5.6.1.1.1 As the test result depends on the used apparatus, it is impossible to give
general parameters for the chromatographic analysis. The following parameters have
been proved to be appropriate for the test. The optimal analysis conditions may be
selected depending on instruments and apparatus

5.6.1.1.2 Chromatographic column: a stainless steel column with a length of 150mm and
an inner diameter of 3.9 mm, with a stationary phase of RP18 whose particle size is 5μm.

5.6.1.1.3 Detection wavelength: 200 nm~700 nm.

5.6.1.1.4 Quantitative wavelength: 400 nm, 500 nm, 540 nm, 590 nm and 620 nm.

5.6.1.1.5 Flow rate: 0.8 mL/min.

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