SN/T 5143-2019 in English

VALID

Determination of semicarbazide in flour and its products for export-LC-MS/ MS method

Issued on:2019-10-25
Implemented on:2020-05-01
File Format:PDF
Delivery:Via email within 1~3 business days

Price(USD)： $240.00
$233.00

Standard No:	SN/T 5143-2019
Document status:	VALID
Title in English:	Determination of semicarbazide in flour and its products for export-LC-MS/ MS method
Title in Chinese:	出口小麦粉及其制品中氨基脲的测定液相色谱-质谱/质谱法
Language:	English
File Format:	Electronic (PDF)
Delivery:	Via email within 1~3 business days
Issued on:	2019-10-25
Implemented on:	2020-05-01
Professional Classification:	SN-Import&Export Inspection
Related Keywords:	isotope internal standard method low derivatization efficiency method principle export-lc-ms/ ms method introduction analysis traditional method method performance indicators limit
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Introduction

Analysis of the core content of the standard

This standard specifies the method principle for detecting the residue of semicarbazide in flour and its products using liquid chromatography-tandem mass spectrometry: semicarbazide in the sample is derivatized with o-nitrobenzaldehyde under acidic conditions, and after purification by HLB solid phase extraction column, quantitative analysis is carried out using multiple reaction monitoring mode (MRM).

Key instrument parameters

Instrument module	Parameter setting	Technical requirements
Chromatographic column	Waters BEH C18 (50mm×2.1mm,1.7μm)	Column temperature: 30℃
Mobile phase	0.1% formic acid aqueous solution-acetonitrile gradient elution	Flow rate: 0.3mL/min
Mass spectrometry conditions	ESI positive ion mode	Collision energy: 10eV

Method performance indicators

Limit of quantification (LOQ): 0.5μg/kg
Recovery range: 73%-112%
Precision (RSD): ≤15.69%(n=10)

Key steps of sample pretreatment

Derivatization reaction: Add 50μL isotope internal standard, 10mL 0.2mol/L hydrochloric acid solution, and 100μL 0.1mol/L o-nitrobenzaldehyde methanol solution to 2g sample, and react at 37℃ for 16 hours
Purification process: Use HLB column (60mg/3mL), elute with 6mL water and 3mL ethyl acetate in sequence
Filter membrane selection: 0.22μm organic filter membrane filtration

Comparison of technological evolution

Detection items	This method (LC-MS/MS)	Traditional method (GC-MS)
Sensitivity	0.5μg/kg	5μg/kg
Analysis time	10min/sample	30min/sample
Anti-interference ability	MRM mode double confirmation	Single ion monitoring

Implementation Suggestions

Key Points for Quality Control

Each batch of samples should include blank controls and spike recovery experiments
The derivatization reaction requires strict temperature control (37±1℃)
The retention time deviation of the chromatographic peak should be controlled within ±2.5%

Solutions to Common Problems

Matrix effect: Correct with isotope internal standard method
Low derivatization efficiency: Check the storage conditions of the o-nitrobenzaldehyde reagent (protected from light at 4℃)
Abnormal recovery rate: Reactivate the HLB column (3mL methanol + 3mL water)

More samples: NB/T 47013.2-2015 GB 18306-2015 DL/T 368-2010

Sample only — not a preview of SN/T 5143-2019

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