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Basic data
| Standard ID | SN/T 5236-2020 (SN/T5236-2020) |
| Description (Translated English) | (Import and export textiles Determination of harmful dyes Liquid chromatography-high resolution mass spectrometry) |
| Sector / Industry | Commodity Inspection Standard (Recommended) |
| Classification of Chinese Standard | W04 |
| Classification of International Standard | 59.080.01 |
| Word Count Estimation | 18,124 |
| Date of Issue | 2020-08-27 |
| Date of Implementation | 2021-03-01 |
| Regulation (derived from) | General Administration of Customs Announcement No. 98 [2020] |
| Issuing agency(ies) | General Administration of Customs |
SN/T 5236-2020: (Import and export textiles Determination of harmful dyes Liquid chromatography-high resolution mass spectrometry)
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
Issued by the General Administration of Customs of the People's Republic of China
2020-08-27 release
2021-03-01 implementation
Textiles for import and export-Determination of harmful dyestuffs-
Liquid chromatography-high resolution mass spectrometry method
Replace SN/T 3011.1-2011
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
Please note that some of the contents of this document may involve patents. Publication of this document
The agency is not responsible for identifying these patents.
This standard was proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organizations of this standard. Qingdao Customs of the People's Republic of China, Chinese Academy of Inspection and Quarantine Sciences, Shenzhen
customs.
The main drafters of this standard. Luo Xin, Niu Zengyuan, Ye Xiwen, Tang Zhixu, Chen Jing, Ma Qiang, Xie Tangtang, Wang Jianhua, Liu Jingjing.
Determination of harmful dyes for import and export textiles
Liquid chromatography-high resolution mass spectrometry
Warning. The personnel using this standard should have practical experience in formal laboratory work. This standard does not point out all possible safety issues
question. 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 the use of liquid chromatography-high resolution mass spectrometry (LC-HRMS) for the simultaneous determination of 46 hazardous dyes in textile products.
method.
This standard applies to the determination of 46 harmful dyes in textile products processed by printing and dyeing.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
3 Principle
The sample was heated and extracted with pyridine-aqueous solution as the extraction solvent, the supernatant was diluted, and then liquid chromatography-high resolution mass spectrometry
(LC-HRMS) determination, external standard method quantification.
4 Reagents and materials
Unless otherwise stated, all reagents used are of analytical grade. The water is the first grade water that meets the requirements of GB/T 6682.
4.1 Acetonitrile. chromatographically pure.
4.2 Methanol. chromatographically pure.
4.3 Pyridine. excellent grade pure.
4.4 Ammonium acetate. chromatographically pure.
4.5 Formic acid. chromatographically pure.
4.6 Aqueous solution of ammonium acetate (0.385 g/L). accurately weigh 0.385 g of ammonium acetate (4.4) and dissolve in water, and transfer to a 1000 mL volumetric flask.
Constant volume with water.
4.7 Ammonium acetate aqueous solution (0.385 g/L, containing 0.01% formic acid). accurately weigh 0.385 g of ammonium acetate (4.4) and dissolve in water, and add 100 μL
Formic acid (4.5), transfer to a 1000 mL volumetric flask, and dilute to volume with water.
4.8 Pyridine-aqueous solution (11, volume ratio). equal volume of pyridine (4.3) is mutually soluble in water and stored in a brown glass bottle.
4.9 Methanol-aqueous solution (11, volume ratio). equal volume of methanol (4.2) and water are mutually soluble.
4.10 46 kinds of dye standards. see Appendix A.
4.11 Standard stock solution. accurately weigh an appropriate amount of dye standard and dissolve it with the solvent listed in Appendix A to make an effective concentration of 100 mg/L
Standard stock solution. The validity period of the standard stock solution is 12 months when stored in a refrigerator at -18 ℃ and protected from light.
4.12 Mixed standard working solution. accurately pipette an appropriate amount of standard stock solution and use methanol-aqueous solution (4.9) to prepare a concentration of 1 mg/L
The mixed standard working solution of, or the standard working solution of other concentration can be prepared as needed. Stored in the refrigerator at -18 ℃ and protected from light,
The validity period of the standard working solution is 1 month.
5 Apparatus and equipment
5.1 Liquid Chromatography-High Resolution Mass Spectrometer (LC-HRMS). Distributed Spray Ion Source (ESI).
5.2 Heating source. equipment that can generate a heat source of (100±2)°C, such as a water bath placed on an electric hot plate and heated to boiling.
5.3 Glass sample bottle. 40 mL with screw cap (with PTFE gasket).
5.4 Electronic balance. Sensitivity 0.01 g and 0.1 mg.
5.5 Microporous membrane. 0.22 μm, polytetrafluoroethylene.
6 Analysis steps
6.1 Sample preparation and extraction
Take a representative sample, cut into pieces of about 5 mm × 5 mm, and mix well. Accurately weigh 1 g (accurate to 0.01 g) sample at 40
Add 20 mL of pyridine-water mixed solution (4.8) to the mL glass bottle (5.3), and extract at (100 ± 2) °C for 35 min. After the extraction is complete,
Cool to room temperature, take the supernatant and dilute 10 times with methanol-water mixed solution (4.9), pass through a 0.22 μm microporous membrane, and wait for the instrument to inject the sample.
6.2 Instrument measurement
6.2.1 Instrumental analysis conditions
6.2.1.1 Liquid chromatography conditions
6.2.1.1.1 Chromatographic column. CAPCELL PAK UG120 C181), 3 μm, 2.0 mm × 100 mm, or equivalent;
6.2.1.1.2 Mobile phase. In positive ion mode. A is 5 mmol/L ammonium acetate aqueous solution (containing 0.01% formic acid) (4.7), B
It is acetonitrile (4.1); in negative ion mode. A is 5 mmol/L ammonium acetate aqueous solution (4.6), and B is acetonitrile (4.1). Positive and negative ion mode
The gradient elution procedure is the same, see Table 1;
6.2.1.1.3 Flow rate. 0.25 mL/min;
6.2.1.1.4 Injection volume. 5 μL;
6.2.1.1.5 Column temperature. 30 ℃.
6.2.1.2 High resolution mass spectrometry conditions
6.2.1.2.1 Ion source. electrospray ion source;
1) This information is given for the convenience of users of this standard, and does not mean approval of the product. If other equivalent products have the same effect,
These equivalent products can then be used.
6.2.1.2.2 Scan mode. positive and negative ion mode, collect separately;
6.2.1.2.3 Detection mode. first level full scan (Full Scan) second level data dependence scan (DDA);
6.2.1.2.4 See Appendix B for other mass spectrometry conditions.
Note. Because the test results are related to the instrument and conditions used, it is impossible to give general parameters for instrument analysis. The use of the above parameters has been proven
It is suitable for testing.
6.3 Qualitative analysis
Under 6.2.1 chromatographic mass spectrometry conditions, please refer to Figure C.1 in Appendix C for the extracted ion chromatograms of the primary precursor ions of each dye standard solution
And Figure C.2.If the retention time of the chromatographic peak of the sample solution is consistent with that of the dye standard working solution (the allowable deviation is within ±0.1 min),
And the deviation between the accurate mass of the precursor ion and the accurate mass of the product ion and the theoretical value is less than or equal to 5 ppm (5×10-6), the sample can be determined
There are corresponding harmful dyes in the product.
6.4 Quantitative analysis
6.4.1 Drawing of calibration curve
According to the testing needs, use the standard working solution to inject samples separately, with the concentration of the standard working solution as the abscissa and the peak area as the ordinate
Mark and draw a calibration curve.
6.4.2 Test solution determination
Use the test solution to inject samples separately to obtain the target peak area. Calculate the content (mg/kg) of each dye in the sample to be tested according to the calibration curve.
The response value of the dye to be tested in the sample should be within the linear range of the method.
6.5 Blank test
Do a blank test with the sample.
7 Result calculation
The harmful dye content in the sample is calculated according to formula (1). The calculation result needs to deduct the blank value.
8 Low limit of determination, recovery and precision
8.1 Lower limit of determination
The lower limit of the determination range of this method is 0.01 mg/kg ~10 mg/kg. Please refer to Appendix D for the specific values of each compound.
8.2 Recovery rate
See Appendix E.
8.3 Precision
Under repeatability conditions, the absolute difference between two independent determination results is not more than 15% of the arithmetic mean; under repeatability conditions,
The absolute difference between the results of the two laboratories is not more than 20% of the arithmetic mean.
9 Test report
The test report should at least give the following contents.
a) Sample source and description;
b) Instruments and standards used;
c) Test results;
d) Any details that deviate from this standard;
e) Test date.
Appendix A
(Informative appendix)
46 harmful dyes
Table A.1 Information about 46 dye compounds
Appendix B
(Informative appendix)
46 dyes LC-HRMS conditions 1)
B.1 Primary scan resolution. R=70 000 (FWHM at m/z.200).
B.2 Secondary scanning resolution. R=17 500 (FWHM at m/z.200).
B.3 First-level scanning scanning range. m/z 150～1 000.
B.4 Spray voltage. 3.5 kV for positive ion mode and -2.9 kV for negative ion mode.
B.5 S-lens RF level. 50 V for positive ion mode and -50 V for negative ion mode.
B.6 Capillary temperature. 320 ℃.
B.7 Sheath gas (N2) pressure. 2.76 × 10
5 Pa (ie 40 arb).
B.8 Auxiliary gas (N2) flow rate. 3.33 L/min (that is, 10 arb).
B.9 Atomizing gas temperature. 300 ℃.
B.10 Collision mode...
...
