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Basic data
| Standard ID | SN/T 5235-2020 (SN/T5235-2020) |
| Description (Translated English) | Textiles for import and export - Determination of the residual content of 19 Liquid chromatography-mass spectrometry method |
| Sector / Industry | Commodity Inspection Standard (Recommended) |
| Classification of Chinese Standard | W04 |
| Classification of International Standard | 59.080.01 |
| Word Count Estimation | 10,115 |
| 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 5235-2020: Textiles for import and export - Determination of the residual content of 19 Liquid chromatography-mass spectrometry method
---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.
Textiles for import and export-Determination of the residual content of 19
chlorinated phenols-
Liquid chromatography- mass spectrometry method
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
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
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, Qingdao Product Quality Supervision and Inspection Institute, China Inspection and Quarantine
Academy of Sciences.
The main drafters of this standard. Gao Yonggang, Niu Zengyuan, Sun Li, Ye Xiwen, Zhang Yanyan, Ma Qiang, Wang Xin, Gao Xuhui, Qu Jingwu,
Alpine.
19 kinds of chlorinated phenol residues in import and export textiles
Determination of residue liquid chromatography-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-mass spectrometry (LC-MS) for the determination of 19 chlorophenols in textiles (see Appendix A).
Set method.
This standard is applicable to the determination of 19 chlorophenols in various textile materials and products.
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 Principles of the method
The sample is extracted with methanol, after concentration, the methanol is fixed to volume, and the liquid chromatography-mass spectrometer (LC-MS) is used for the determination. The external standard method
Quantitative.
4 Reagents and materials
Unless otherwise specified, all reagents are of analytical grade, and the experimental water is first-grade water that meets the requirements of GB/T 6682.
4.1 Methanol. chromatographically pure.
4.2 Acetic acid. chromatographically pure.
4.3 Standards of chlorinated phenol. see Appendix A, purity ≥ 98%.
4.4 Ammonium acetate. chromatographically pure.
4.5 5 mmol/L ammonium acetate solution (containing 0.4% acetic acid). Weigh 0.385 g ammonium acetate (4.4), pipette 4.0 mL acetic acid (4.2), and use water
Dissolve and dilute to 1 000 mL, shake well and set aside.
4.6 1 000 mg/L standard stock solution. accurately weigh 0.025 g (accurate to 0.1 mg) of each phenol standard into a 25 mL volumetric flask,
Dilute the alcohol (4.1) to the mark, mix well, and store in a brown bottle. Store in a refrigerator at 0 ℃ ~ 4 ℃. The validity period is 6 months.
4.7 Standard working solution. Prepare a standard working solution of appropriate concentration or composition as required.
5 Apparatus and equipment
5.1 Liquid chromatography-mass spectrometer (LC-MS). equipped with electrospray ionization source (ESI).
5.2 Analytical balance. Sensitivity is 0.1 mg and 1 mg.
5.3 Ultrasonic generator. frequency 40 kHz.
5.4 Rotary evaporator.
5.5 Sample bottle. 40 mL.
5.6 Heart bottle. 100 mL.
5.7 Syringe. 2 mL.
5.8 Organic filter membrane. 0.22 μm.
6 Test procedure
6.1 Sample preparation
Take a representative sample, cut it into small pieces below 5 mm × 5 mm, and mix well.
6.2 Extraction
Weigh 1.0 g (accurate to 1 mg) sample, place it in a sample bottle (5.5), add 20 mL of methanol (4.1) and mix well, then place it at room temperature
After 20 minutes of ultrasonic extraction, the extract was poured into a chicken heart flask (5.6), and the sample residues were extracted with 20 mL of methanol (4.1) ultrasonically, and then combined
The extract is placed in a chicken heart bottle (5.6), concentrated to near dryness with a rotary evaporator (5.4), dilute to 1 mL with methanol (4.1), and mix well.
After filtration with organic filter membrane (5.8), it is measured by high performance liquid chromatography-mass spectrometer.
6.3 Blank test
Carry out a blank test with the same product.
6.4 Determination
6.4.1 Measurement conditions
Since the test results depend on the instrument used, it is impossible to give general parameters for liquid chromatography analysis. The set parameters should ensure
During chromatographic determination, the measured component can be effectively separated from other components. The following parameters are proved to be feasible.
a) Chromatographic column. Poroshell 120 SB-C18, 2.1 mm×100 mm (inner diameter), particle size 2.7 μm or equivalent.
b) Column temperature. 40 ℃.
c) Mobile phase. ammonium acetate solution (4.5) methanol (4.1), the gradient elution procedure is shown in Table 1.
6.4.2 Qualitative analysis
Under the same test conditions, use liquid chromatography-mass spectrometer to measure the standard working solution and sample solution separately.
The retention time of the mass chromatographic peak is consistent with that of the standard working solution (within ±2.5%), and the target compound in the sample spectrum
The relative abundance of the qualitative ion pair of the substance is compared with the relative abundance of the corresponding qualitative ion pair in the spectrum of a standard solution with a close concentration, such as
If the relative abundance deviation does not exceed the range specified in Table 2, it can be determined that the corresponding analyte exists in the sample.
6.4.3 Quantitative analysis
Measure the sample liquid to be tested according to the measurement conditions in 6.4.1, and quantify by external standard method. The response value of chlorophenol in the sample solution to be tested should be in the standard
Within the linear range of the curve (see Appendix C), if it exceeds the linear range, it should be diluted before analysis.
7 Result calculation
Calculate the content of various phenolic compounds in the sample according to formula (1), and keep the calculation result to 2 decimal places.
Xi - the content of chlorophenol compound i in the sample, in milligrams per kilogram (mg/kg);
Ai --the chromatographic peak area of the chlorophenol compound i in the sample solution;
Ai0 --the chromatographic peak area of the chlorophenol compound i in the blank solution;
Ci-the concentration of chlorophenol compound i in the standard working solution, in milligrams per liter (mg/L);
Ais-the chromatographic peak area of the chlorophenol compound i in the standard working solution;
8 Low limit of determination
The lower limit of the determination of chlorinated phenol compounds in this standard is 0.05 mg/kg.
9 Recovery rate and precision
9.1 Recovery rate
The average recovery rate of this standard for 19 kinds of chlorinated phenol compounds at the concentration levels of 0.05 mg/L, 0.5 mg/L and 5.0 mg/L
80.3%～103.5%.
9.2 Precision
In the same laboratory, the same operator uses the same equipment and according to the same test method to continuously perform the same test on the same object.
Independent test, the relative standard deviation of the two independent test results obtained is not more than 10%. With the arithmetic greater than these two measured values
It is assumed that 10% of the average value does not exceed 5%.
10 Test report
The test report should at least provide the following.
a) Sample source and description;
b) Test method used;
c) Test results;
d) Any details that deviate from this standard;
e) Test date.
Appendix A
(Normative appendix)
Appendix B
(Informative appendix)
19 reference conditions for chlorophenol mass spectrometry
See Table B.1.
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