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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 National Textile and Apparel Council.
This standard is under the jurisdiction of the National Technical Committee 209 on Textiles of Standardization Administration of China (SAC/TC 209).
Textiles - Determination of neonicotinoid pesticide residues
Warning - Persons using this standard shall be familiar with normal laboratory practice. 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 method for determining seven kinds of neonicotinoid pesticide residues in textiles with a liquid chromatograph mass spectrometer (LC-MS/MS).
This standard is applicable to various textiles.
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 Water for analytical laboratory use - Specification and test methods
3 Principle
Extract specimens using acetonitrile ultrasonic, filter the extracting solution by membrane, then determine and confirm by LC-MS/MS, and quantify by external standard method.
4 Reagents and materials
4.1 Acetonitrile: chromatographically pure.
4.2 Seven kinds of standard neonicotinoid pesticides: purity≥98%, see Annex A.
4.3 Standard stock solution (about 1,000mg/L): accurately weigh appropriate standard neonicotinoid pesticides (accurate to 0.000 1g) respectively, and use acetonitrile (4.1) to prepare standard stock solution of each pesticide with a mass concentration of about 1,000mg/L.
Note: The standard stock solutions are valid for 12 months if stored at 0~4℃ in a dark place.
4.4 Mixed standard working solutions (about 10mg/L): accurately pipette appropriate standard stock solutions (4.3), use acetonitrile (4.1) to prepare mixed standard working solution with a concentration of about 10mg/L, and then prepare standard working solutions with other concentrations as required.
Note: The mixed standard working solutions are valid for 3 months if stored at 0~4℃ in a dark place.
4.5 Water: Class-II water complying with GB/T 6682.
5 Instruments and apparatus
5.1 Liquid chromatograph mass spectrometer (LC-MS/MS): equipped with electrospray ionization (ESI) source.
5.2 Ultrasonic generator: with an operating frequency of 40kHz.
5.3 Balances: with a sensitivity of 0.000 1g and 0.01g respectively.
5.4 Conical flask: with a ground stopper, and a capacity of 100mL.
5.5 PTFE filter membrane: with a pore diameter of 0.22μm.
6 Analysis procedures
6.1 Extraction
Take a representative sample, cut it into pieces smaller than 5mm×5mm, and then mix them uniformly. Weigh 1.0g (accurate to 0.01g) mixed specimen, put it in a conical flask (5.4), add 20mL acetonitrile (4.1) accurately, insert the stopper, put the conical flask in an ultrasonic generator (5.2) for extraction at room temperature for 60min, and filter the sample solution into the sample flask with a PTFE filter membrane (5.5) for LC-MS/MS analysis.
6.2 Determination
6.2.1 Liquid chromatography conditions
As the test result depends on the instruments adopted, it is impossible to provide the general parameters for chromatographic analysis, and the following parameters are proved applicable to the test:
a) chromatographic column: ZORBAX SB-C18, 2.1mm×150mm, 3.5μm, or equivalent;
b) flow velocity: 0.2mL/min;
c) column temperature: 40℃;
d) injection volume: 1μL;
e) mobile phase: A is water and B is acetonitrile;
f) gradient elution procedure: see Table 1.
Contents
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Instruments and apparatus
6 Analysis procedures
7 Result calculation and expression
8 Lower determination limit and precision
9 Test report
Annex A (Normative) List of seven kinds of neonicotinoid pesticides
Annex B (Informative) Mass spectrometry conditions
Annex C (Informative) Total ion chromatogram of mixed standard solutions of seven kinds of neonicotinoid pesticides by liquid chromatography-tandem mass spectrometry
