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GB/T 39076-2020: Textiles - Determination of neonicotinoid pesticide residues Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid
Similar standardsGB/T 39076-2020: Textiles - Determination of neonicotinoid pesticide residues---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT39076-2020GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 59.080.01 W 04 Textiles - Determination of neonicotinoid pesticide residues ISSUED ON: JULY 21, 2020 IMPLEMENTED ON: FEBRUARY 01, 2021 Issued by: State Administration for Market Regulation; Standardization Administration of PRC. Table of ContentsForeword ... 3 1 Scope ... 4 2 Normative references ... 4 3 Principles ... 4 4 Reagents and materials ... 4 5 Apparatus and equipment ... 5 6 Analytical procedures ... 5 7 Calculation and presentation of results ... 7 8 Low limit of determination and precision ... 8 9 Test report ... 8 Appendix A (Normative) List of 7 neonicotinoid pesticides ... 10 Appendix B (Informative) Mass spectrometry conditions ... 11 Appendix C (Informative) Total ion chromatograms of liquid chromatography- tandem mass spectrometry mixed standard solutions of 7 neonicotinoid pesticides ... 12 Textiles - Determination of neonicotinoid pesticide residues Warning - The personnel using this standard shall have practical experience in formal laboratory work. This standard does not point out all possible safety issues. It is the user's responsibility to take appropriate safety and health measures, and to ensure compliance with the conditions stipulated by relevant national laws and regulations.1 ScopeThis standard specifies the method of use of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of 7 neonicotinoid pesticide residues in textiles. This standard applies to all types of textile products.2 Normative referencesThe following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) are applicable to this standard. GB/T 6682 Water for analytical laboratory use - Specification and test methods3 PrinciplesThe specimen is ultrasonically extracted by acetonitrile; the extract is filtered through a filter membrane, then measured and confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS), quantified by external standard method.4 Reagents and materials4.1 Acetonitrile: Chromatographically pure. 4.2 The 7 standard neonicotinoid pesticides: purity ≥ 98%, as shown in Appendix A. 4.3 Standard stock solution (approximately 1000 mg/L): Respectively accurately weigh appropriate amounts of neonicotinoid pesticide standard products (accurate to 0.0001 g). Use acetonitrile (4.1) to prepare each substance to the standard stock solution which has a mass concentration of approximately 1000 mg/L. Note: When stored at 0 °C ~ 4 °C in the dark, the validity period of the standard stock solution is 12 months. 4.4 Mixed standard working solution (approximately 10 mg/L): Accurately pipette an appropriate amount of standard stock solution (4.3). Use acetonitrile (4.1) to prepare a mixed standard working solution which has a concentration of approximately 10 mg/L. Then, prepare the standard working solution of other concentrations as needed. Note: When stored at 0 °C ~ 4 °C in the dark, the validity period of the mixed standard working solution is 3 months. 4.5 Water: Class II water that meets the requirements of GB/T 6682.5 Apparatus and equipment5.1 Liquid chromatography-tandem mass spectrometer (LC-MS/MS): It is equipped with electrospray ionization source (ESI). 5.2 Ultrasonic generator: The working frequency is 40 kHz. 5.3 Balance: Sensitivity is 0.0001 g and 0.01 g, respectively. 5.4 Conical flask: It has a ground stopper; the capacity is 100 mL. 5.5 Polytetrafluoroethylene filter membrane: The pore size is 0.22 μm.6 Analytical procedures6.1 Extraction Take a representative sample. Cut it into small pieces below 5 mm × 5 mm. Mix well. Weigh 1.0 g (accurate to 0.01 g) and mix the specimen uniformly. Place it in a conical flask (5.4). Accurately add 20 mL of acetonitrile (4.1). Close the stopper. Place the conical flask in the ultrasonic generator (5.2). Extract it at room temperature for 60 minutes. Use polytetrafluoroethylene filter membrane (5.5) to filter the sample solution into a sample bottle, which is used for LC- MS/MS analysis. Where: Xi - The content of neonicotinoid pesticide i in the specimen, in milligrams per kilogram (mg/kg); ci - The concentration of neonicotinoid pesticide i in the sample as calculated from the standard curve, the unit is milligrams per liter (mg/L); V - Volume of sample liquid, the unit is milliliters (mL); F - Dilution factor; m - The mass of the specimen, in grams (g). 7.2 Results presentation The test results are represented by the test results of various neonicotinoid pesticides. The calculation results are kept to one decimal place. When it is below the lower limit of determination, the test result is "not detected".8 Low limit of determination and precision8.1 Lower limit of determination The lower limit of determination is 0.2 mg/kg. 8.2 Precision In the same laboratory, when the same operator uses the same equipment, according to the same test method, to carry out tests of same tested object independently in a short time, at the 95% confidence level, the absolute difference of the two independent test results obtained is not more than 20% of the arithmetic mean of the two measured values.9 Test reportThe test report shall give at least the following contents: a) Sample description; b) Number of this standard; c) Test results; ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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