SN/T 4673-2016 in English

VALID

Determination of ethephon,thidiazuron,diuron pesticides residues 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
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Standard No:	SN/T 4673-2016
Document status:	VALID
Title in English:	Determination of ethephon,thidiazuron,diuron pesticides residues in cotton for import and export―Liquid chromatography-tandem mass spectrometry method
Title in Chinese:	进出口棉花中乙烯利、噻苯隆、敌草隆农药残留量的测定液相色谱一质谱/质谱法
Language:	English
File Format:	Electronic (PDF)
Delivery:	Via email within 1~3 business days
Issued on:	2016-12-12
Implemented on:	2017-07-01
Professional Classification:	SN-Import&Export Inspection
Related Topics:	No peak in liquid chromatography Liquid chromatography does not show Styrene liquid chromatography No peak in mass spectrum Pharmacokinetic mass spectrometry liquid chromatography mass spectrometry diquat Styrene Mass Spectrometry Imported liquid chromatography No peak in mass spectrum No peak in liquid chromatography Styrene Mass Spectrometry prodrug, mass spectrometry as 4673 cotton spectrum cotton Mass Spectrometry Liguron Mass Spectrometry Styrene Mass Spectrometry Detection MS mass 18 mass spectrometry The peak of benzene in the mass spectrum Gas chromatography mass spectrometry ethylene Determination of styrene in construction adhesives for import and export - Gas chromatography-mass spectrometry LC-MS co-elution Liquid chromatography + peak extraction Liquid chromatography peaks within a few minutes at the earliest Liquid chromatography peaks in 70 minutes Imported chromatography Liquid chromatography peaks in one minute Quantification by mass spectrometry MS co-elution Improvements in mass spectrometry Mass Spectrometry Liquid Chromatography Peak Styrene liquid chromatography Styrene liquid chromatography Absolute quantitation by mass spectrometry LC outlet ring Quantification by mass spectrometry Pesticide residue chromatographic peak front Mass Spectrum of Ethylbenzene Ethylbenzene Mass Spectrometry Pesticide Residue Mass Spectrometry Detection Absolute quantitation by mass spectrometry drug mass spectrometry cycloalkene mass spectrometry Mass Spectrum 41 Peak Imported gas chromatograph drug mass spectrometry Liquid Chromatography Styrene Drug mass spectrometry detection Styrene Liquid Chromatography Styrene mass spectrum peak Mass spectrometry Gas Chromatography-Mass Spectrometry of Pesticide Residues in Water Styrene liquid phase in water Acetic acid liquid chromatography mass spectrometry Chromatographic determination of styrene Mobile phase for mass spectrometry Traditional Chinese medicine mass spectrometry Pesticide liquid chromatography data Liquid chromatography method for detecting pesticide residues in agricultural products

本标准规定了进出口棉花中乙烯利、噻苯隆、敌草隆农药残留量的液相色谱-质谱/质谱法。

Introduction

Technical Interpretation of the Standard

SN/T 4673-2016 establishes a method for the detection of three plant growth regulators (ethephon, thiazuron, and diuron) residues in cotton using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Method validation demonstrated recoveries between 80% and 110%, with relative standard deviations (RSDs) ≤15%, meeting the requirements of the Codex Alimentarius Commission (CAC) for pesticide residue analysis.

Comparison of method principles

Detection indicators

Pretreatment method

Chromatographic conditions

Mass spectrometry parameters

Ethephon

Phosphate buffer extraction

C8 chromatographic column (150mm×4.6mm)

Precursor ion m/z 142.7, product ion m/z 107.0/79.3

Thidiazuron

Ultrasound-assisted extraction

Mobile phase: methanol-water (6+4)

Precursor ion m/z 219.2, product ion m/z 1. Sample pretreatment: The cotton sample was ground into 2 mm particles using a freeze grinder. Phosphate buffer (pH=8) was used as the extraction solvent. The extraction was carried out at 300 r/min with shaking for 20 min. The sample was filtered through a 0.22 μm organic filter membrane and then tested on an analyzer. 2. Mass Spectrometry Optimization: In negative electrospray ionization (ESI) mode, collision energies were optimized to -25 V (ethephon), -34 V (thidiazuron), and -17 V (diuron). Multiple Reaction Monitoring (MRM) was used to enhance selectivity. 3. Quality Control: Spiked recoveries were measured in parallel for each batch of samples. The spiked concentrations of ethephon, thidiazuron, and diuron were 100 μg/kg, 40 μg/kg, and 4 μg/kg, respectively. The recoveries were maintained within the range of 70%-120%.

Implementation Recommendations

Laboratories should regularly calibrate the mass axis of the mass spectrometer to ensure that the mass accuracy deviation is ≤0.1Da
Since the cotton matrix is complex, it is recommended to use the isotope internal standard method to compensate for the matrix effect
When the test result is close to the limit standard (e.g., the detection value of diuron is >4μg/kg), it is necessary to increase the number of qualitative ion pairs for confirmation

Standard Evolution Analysis

Compared with the GB/T 19648-2006 method, the innovations of this standard include:
1) Incorporating three pesticides with different functions into the same detection system
2) Using tandem mass spectrometry technology to reduce the detection limit by 10 times
3) Introducing a pH-controlled extraction process to improve the recovery stability of the acidic pesticide ethephon

More samples: NB/T 47013.2-2015 DL/T 368-2010 JJG 21-2008

Sample only — not a preview of SN/T 4673-2016

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