SN/T 4671-2016 in English
VALIDDetermination of glyphosate and its metabolite residue in cotton for import and export―Liquid chromatography-tandem mass spectrometry method
- Issued on:2016-12-12
- Implemented on:2017-07-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$156.00
Introduction
Technical Background of the Standard
This standard, issued on December 12, 2016, and implemented on July 1, 2017, specifies the detection of glyphosate and its metabolites in cotton products using liquid chromatography-tandem mass spectrometry. The technique is based on the FMOCl derivatization reaction and quantitative analysis using an isotope internal standard method, with a detection limit of 0.05 mg/kg.
Core Detection Process
| Steps | Key Parameters | Technical Points |
|---|---|---|
| Sample Pretreatment | 10 g sample was crushed to 2 mm | Derivatization was performed using 1.0 μg/mL isotope internal standard solution |
| Derivatization Reaction | 30 min oscillation reaction | Add 100 μL borate buffer and 50 μL FMOCl reagent |
| Chromatographic Conditions | C18 column (100 mm × 2.1 mm) | Gradient elution: 5 mM ammonium acetate/methanol |
Method Validation Data
Standard validation showed that at spike levels of 0.05-0.20 mg/kg, glyphosate recoveries ranged from 75.2% to 96.4%, and metabolite recoveries ranged from 68.8% to 94.0%. Mass spectrometry detection was performed using a TSQ Quantum ULTRA AM system in positive ESI mode with collision energy optimized to 10-25 V.
Key Points
- Strictly control the storage conditions of the derivatization reagent FMOCl (5°C, protected from light)
- Note the retention time differences of the internal standard (13C15N-labeled compound): glyphosate 9.8 minutes, metabolite 12.7 minutes
- Mass spectrometer parameters need to be calibrated regularly to ensure that the response value deviation is ≤2.5%

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