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