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GB/T 37040-2018 English PDF (GBT37040-2018)

GB/T 37040-2018 English PDF (GBT37040-2018)

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GB/T 37040-2018: Limit and determination of carcinogenic dyes in dye products
This Standard specifies limits and determination methods of 12 carcinogenic dyes (see Annex A) in dye product. This Standard is applicable to various formulations of dye products.
GB/T 37040-2018
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.01;87.060.10
G 55
Limit and determination of carcinogenic dyes in dye
product
ISSUED ON: DECEMBER 28, 2018
IMPLEMENTED ON: NOVEMBER 01, 2019
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Requirements ... 4
4 Principle ... 4
5 Test methods ... 5
6 Minimum detection limit, precision and recovery rate ... 9
7 Test report ... 9
Annex A (normative) Detection wavelength of HPLC-DAD method of
carcinogenic dye and characteristic ion of HPLC-MS method ... 11
Annex B (informative) Schematic diagram of HPLC-DAD method
chromatogram of standard working solution at different detection wavelengths ... 12
Limit and determination of carcinogenic dyes in dye
product
WARNING - The personnel using this Standard shall have practical
experience in formal laboratory work. This Standard does not point out all possible safety issues. The user is responsible for taking appropriate
safety and health measures and ensuring compliance with the conditions
stipulated by relevant national laws and regulations.
1 Scope
This Standard specifies limits and determination methods of 12 carcinogenic dyes (see Annex A) in dye product.
This Standard is applicable to various formulations 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 and expression and judgement of limiting values
3 Requirements
The content of each carcinogenic dye (see Annex A) in the dye product shall not exceed 150mg/kg.
4 Principle
After the sample is dissolved (or extracted), use high performance liquid chromatography-diode array detector (HPLC-DAD) to determine the nature; use peak area external standard method to quantify carcinogenic dyes. For Prepare the single-component carcinogenic dye standard stock methanol
solution listed in Annex A of which the effective concentration is 200mg/L. Store it in the freezer of a refrigerator from light. It shall be valid for 1 year. 5.4.2 Standard working solution
Group A: Take 0.5mL from the basic violet 14 standard stock solution and place it in a 50mL volumetric flask. Use methanol to dilute and set it to a constant volume.
Group B: Respectively take 0.5mL from the remaining 11 standard stock
solutions and place them in 50mL volumetric flasks.
Standard working solution can be prepared into other suitable concentrations as required. Prepare when required.
5.5 Preparation of sample solution
Methanol soluble dye: Weigh 0.5g of sample (to the nearest of 0.0001g). Place it in a 50mL volumetric flask. Use methanol to dissolve. Dilute and set it to a constant volume. Vibrate in an ultrasonic generator. Fully dissolve and make it ready for use.
Methanol insoluble dye: Weigh 0.5g of sample (to the nearest of 0.0001g). Place it in a 100mL conical flask with grinding mouth stopper. Accurately add 50mL of methanol. In an ultrasonic generator, conduct 30min extraction. Cool to room temperature. Use 0.45μm PTFE membrane filter head to filter the extract for use.
5.6 Spectrum analysis
5.6.1 HPLC-DAD analysis method
5.6.1.1 HPLC-DAD chromatographic conditions
5.6.1.1.1 Since the test results depend on the instrument used, it is impossible to give general parameters for chromatographic analysis. The following
parameters have been proved to be suitable for testing. It may, according to different instruments and equipment, select the best analysis conditions. 5.6.1.1.2 Chromatographic column: Stainless steel column of which the length is 150mm, the inner diameter is 3.9mm, the stationary phase is RP18, the particle size is 5μm.
5.6.1.1.3 Detection wavelength: 200nm~700nm.
5.6.1.1.4 Quantitative wavelength: 400nm, 500nm, 540nm, 590nm, 620nm.
Turn on the liquid chromatography-mass spectrometer. After the various
operating conditions of the instrument are stable, use a micro syringe to pipette 20μL of sample solution and standard working solutions A, B to respectively inject into injection valves. After the last component flows out (see Annex B), use chromatography workstation to process the result. Through characteristic ion and comparation on the retention time of the chromatographic peak of the sample and the standard sample, determine the nature.
5.7 Chromatogram
Refer to Annex B for the liquid chromatogram of carcinogenic dyes determined by this method.
6 Minimum detection limit, precision and recovery rate
6.1 Minimum detection limit
The minimum detection limit of each carcinogenic dye in this method is 10mg/kg. 6.2 Precision
In the same laboratory, the same operator uses the same equipment according to the same test method. Within a short time, independently test the same testing object. The absolute difference between the two independent test results obtained is not more than 10% of its arithmetic mean.
6.3 Recovery rate
Use standard addition method. Add 1mL of the standard stock solution to the sample that has been determined by this method not contain carcinogenic dyes. Operate according to Clause 5. The measured recovery rate of carcinogenic dyes shall be 70%~130%.
7 Test report
The test report shall at least give the following information:
a) Sample description;
b) Standard reference number used;
c) Test result;
d) Deviation from standard;
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