Codeofchina.com 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 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 sensitizing 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 requirements and determination methods for 20 types of sensitizing dyes (see Annex A) in dye products.
This standard is applicable to each dosage form of dye products.
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 judgment of limiting values
3 Requirements
The content of all sensitizing dyes (see Annex A) in dye products shall not be greater than 150 mg/kg.
4 Theory
Dissolve out the sensitizing dyes in the dyes with methanol as solvent. Separate and carry out qualitative determination for each sensitizing dye by using the high performance liquid chromatography-diode array detector (HPLC-DAD), and quantify then using the peak area external standard method. Detected and uncertain samples shall be qualitatively determined by liquid chromatography-tandem mass spectrometry (HPLC-MS/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) 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 sensitizing dyes (see Annex A).
5.2.2 Acetonitrile: chromatographically pure.
5.2.3 Methanol: chromatographically pure.
5.2.4 Aqueous sodium acetate solution: 0.01 mol/L.
5.2.5 PTFE film filter head: 0.45 μm.
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 Chromatographic column: a stainless steel column with a length of 150mm and an inner diameter of 3.9 mm, a stationary phase of RP18 and a particle size of 5 μm.
5.3.3 Chromatographic working station or integrator.
5.3.4 Blunt microinjector or automatic sample injector.
5.3.5 Ultrasonic generator.
5.3.6 Ground conical flask with stopper: 150 mL.
5.4 Liquid chromatographic analysis conditions
5.4.1 Flow rate: 0.8 mL/min;
5.4.2 Column temperature: 40 ℃;
5.4.3 Detection wavelength: 200 nm~700 nm;
5.4.4 Quantitative wavelength: 420 nm, 450 nm, 570 nm and 640 nm.
5.4.4 Injection volume: 10μL.
5.4.6 Mobile phase: Organic phase A: acetonitrile; Water phase B: 0.01 mol/L sodium acetate solution. See Table 1 for mobile phase gradient procedure.
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) Information of 20 types of sensitizing dyes
Annex B (Informative) Chromatogram of sensitizing dyes detected by HPLC-DAD method and mass spectrogram detected by HPLC-MS method
Codeofchina.com 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 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 sensitizing 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 requirements and determination methods for 20 types of sensitizing dyes (see Annex A) in dye products.
This standard is applicable to each dosage form of dye products.
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 judgment of limiting values
3 Requirements
The content of all sensitizing dyes (see Annex A) in dye products shall not be greater than 150 mg/kg.
4 Theory
Dissolve out the sensitizing dyes in the dyes with methanol as solvent. Separate and carry out qualitative determination for each sensitizing dye by using the high performance liquid chromatography-diode array detector (HPLC-DAD), and quantify then using the peak area external standard method. Detected and uncertain samples shall be qualitatively determined by liquid chromatography-tandem mass spectrometry (HPLC-MS/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) 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 sensitizing dyes (see Annex A).
5.2.2 Acetonitrile: chromatographically pure.
5.2.3 Methanol: chromatographically pure.
5.2.4 Aqueous sodium acetate solution: 0.01 mol/L.
5.2.5 PTFE film filter head: 0.45 μm.
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 Chromatographic column: a stainless steel column with a length of 150mm and an inner diameter of 3.9 mm, a stationary phase of RP18 and a particle size of 5 μm.
5.3.3 Chromatographic working station or integrator.
5.3.4 Blunt microinjector or automatic sample injector.
5.3.5 Ultrasonic generator.
5.3.6 Ground conical flask with stopper: 150 mL.
5.4 Liquid chromatographic analysis conditions
5.4.1 Flow rate: 0.8 mL/min;
5.4.2 Column temperature: 40 ℃;
5.4.3 Detection wavelength: 200 nm~700 nm;
5.4.4 Quantitative wavelength: 420 nm, 450 nm, 570 nm and 640 nm.
5.4.4 Injection volume: 10μL.
5.4.6 Mobile phase: Organic phase A: acetonitrile; Water phase B: 0.01 mol/L sodium acetate solution. See Table 1 for mobile phase gradient procedure.
Contents of GB/T 36908-2018
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) Information of 20 types of sensitizing dyes
Annex B (Informative) Chromatogram of sensitizing dyes detected by HPLC-DAD method and mass spectrogram detected by HPLC-MS method
