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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 China Petroleum and Chemical Industry Association.
This standard is under the jurisdiction of Technical Committee on Dyestuff of Standardization Administration of China (SAC/TC 134).
Determination of disperse yellow 23 and disperse orange 149 dyes in dye products
Warning: Users of this standard shall be experienced in normal laboratory practicing. 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 determination methods of disperse yellow 23 and disperse orange 149 dyes in dye products.
This standard is applicable to dye products of all dosage forms.
See Annex A for chemical information of disperse yellow 23 and disperse orange 149 dyes.
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
GB/T 8170-2008 Rules of rounding off for numerical values & expression and judgment of limiting values
3 Principle
Extract disperse yellow 23 and disperse orange 149 in dyes with methanol as solvent, separate and qualitatively determine the extracting solution using the high performance liquid chromatography-diode array detector method, and then quantify using the peak area external standard method. Qualitatively determine the detected and uncertain samples using the high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method.
4 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, GB/T 8170-2008.
5 Reagents and materials
5.1 Standard disperse yellow 23 and disperse orange 149 dyes.
5.2 Acetonitrile: chromatographically pure.
5.3 Methanol: chromatographically pure.
5.4 Phosphoric acid.
5.5 Water: filtered with 0.45μm water phase membrane.
5.6 PTFE filter head (pin type filter): 0.45μm.
6 Apparatus
6.1 Liquid chromatograph: infusion pump - with a flow range of 0.1~5.0mL/min, in which the flow stability is ±1%; with a diode array detector (DAD).
6.2 Chromatographic column: a stainless steel column with a length of 150mm and an inner diameter of 4.6mm, with a stationary phase of C18 whose particle size is 5μm.
6.3 Chromatographic working station or integrator.
6.4 Blunt micro-injector or automatic sample injector.
6.5 Ultrasonic generator.
7 Test conditions
7.1 Liquid chromatographic analysis conditions
7.1.1 Flow rate: 0.8mL/min.
7.1.2 Column temperature: 40℃.
7.1.3 Detection wavelength: 200~600nm.
7.1.4 Quantitative wavelength: 380nm, 460nm.
7.1.5 Injection volume: 20μL.
7.1.6 Mobile phase: organic phase A——acetonitrile; aqueous phase B——0.1% phosphoric acid solution.
See Table 1 for mobile phase gradient procedure.
Table 1 Mobile phase gradient procedure
Time/min Mobile phase A/% Mobile phase B/%
0 30 70
3 30 70
5 70 30
30 70 30
32 30 70
40 30 70
As the test result depends on the instruments adopted, it is impossible to provide the general parameters for chromatographic analysis. The above parameters are proved applicable to the test.
7.2 Parameters of liquid chromatography-mass spectrometer (LC-MS/MS) method
7.2.1 Chromatographic column: a stainless steel column with a length of 50mm and an inner diameter of 2.0mm, a stationary phase of C18 whose particle size is 4.0μm.
7.2.2 Flow rate: 0.6mL/min.
7.2.3 Column temperature: 40℃.
7.2.4 Detector: mass selective detector.
7.2.5 Injection volume: 5μL.
7.2.6 Mobile phase: organic phase A——acetonitrile; aqueous phase B——0.1% phosphoric acid solution.
See Table 2 for mobile phase gradient procedure.
Foreword i
1 Scope
2 Normative references
3 Principle
4 General requirements
5 Reagents and materials
6 Apparatus
7 Test conditions
8 Test procedures
9 Result calculation
10 Chromatogram
11 Minimum detection limit, precision and recovery rate
12 Test report
Annex A (Normative) Chemical information of disperse yellow 23 and disperse orange
Annex B (Informative) Chromatograms of disperse yellow 23 and disperse orange 149 dyes using HPLC/DAD and LC-MS/MS methods
