SN/T 5448-2022 in English

VALID

Determination of nitrapyrin pesticide and metabolites residues in foods of plant origin for export Gas chromatography-tandem mass spectrometry method

Issued on:2022-03-14
Implemented on:2022-10-01
File Format:PDF
Delivery:Via email within 1~3 business days

Price(USD)： $250.00
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Standard No:	SN/T 5448-2022
Document status:	VALID
Title in English:	Determination of nitrapyrin pesticide and metabolites residues in foods of plant origin for export Gas chromatography-tandem mass spectrometry method
Title in Chinese:	出口植物源性食品中三氯甲基吡啶及其代谢物的测定气相色谱-质谱/质谱法
Language:	English
File Format:	Electronic (PDF)
Delivery:	Via email within 1~3 business days
Issued on:	2022-03-14
Implemented on:	2022-10-01
Professional Classification:	SN-Import&Export Inspection
Related Keywords:	chromatography-tandem mass spectrometry method introduction interpretation method technical dimension traditional method improvement chromatography-triple quadrupole mass spectrometry purification method solid phase extraction column psa+c18+gcb method derivatization efficiency reaction
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Introduction

Interpretation of the core technology of the standard

This standard uses gas chromatography-triple quadrupole mass spectrometry combined with QuEChERS pretreatment technology to establish a detection system for trichloromethylpyridine and its metabolite 6-chloropyridine-2-carboxylic acid in 8 types of plant-derived foods. The quantitative limit of the method is 0.01-0.05 mg/kg, and the recovery rate is stable in the range of 80%-113%.

Analysis of the innovative points of the method

Technical dimension	Traditional method	Improvement of this method
Derivatization efficiency	Reaction at room temperature for 24h	Accelerated to 30min at 55℃
Purification method	Solid phase extraction column	PSA+C18+GCB composite purification
Matrix effect control	External standard quantification	Matrix-matched internal standard calibration

Key Operation Points

The pH value needs to be strictly controlled during the acidic acetonitrile extraction stage (the amount of formic acid added is 0.1mL), and different matrixes require differentiated pre-treatment:

High-moisture samples (lettuce/citrus): direct extraction

Dry samples (wheat/corn): 15g of sea sand needs to be added to absorb water

In the derivatization reaction, concentrated sulfuric acid needs to be added slowly in an ice bath to prevent local overheating and degradation of the target.

International Compliance Analysis

The method validation data meets the requirements of the EU SANTE/11312/2021 guidelines, especially for:

Six addition levels were used to verify linearity (0-0.4mg/L)
Three pairs of monitoring ions were set to ensure qualitative reliability
The recovery range complies with CODEX CAC/GL 40-1993

Implementation Recommendations

Note for laboratory operation:

The standard substance should be stored at -18℃ and protected from light, CAS No. 1929-82-4 (trichloromethylpyridine)
The chromatographic column is recommended to use a 35% phenyl-polysiloxane stationary phase
During nitrogen blowing and concentration, the temperature is controlled at 40±2℃ to prevent the target substance from volatilizing

More samples: JC/T 2453-2018 YD/T 3934-2021 JJG 21-2008

Sample only — not a preview of SN/T 5448-2022

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