SN/T 5148-2019 in English

VALID

Determination of clonidine and cyproheptadine residues in foodstuffs of animal origin for export LC- MC/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
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Standard No:	SN/T 5148-2019
Document status:	VALID
Title in English:	Determination of clonidine and cyproheptadine residues in foodstuffs of animal origin for export LC- MC/MS method
Title in Chinese:	出口动物源食品中可乐定和赛庚啶残留量的测定液相色谱-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 Topics:	No peak in liquid chromatography Liquid chromatography does not show No peak in mass spectrum Determination of phenolphthalein and emodin in export health food by liquid chromatography-mass spectrometry/mass spectrometry No peak in mass spectrum mass spectrometry semi-quantitative semi-quantitative mass spectrometry No peak in liquid chromatography quantitative mass spectrometry Quantity measured by mass spectrometry mass spectrometry semi-quantitative Substance mobile phase semi-quantitative mass spectrometry Mass Spectrometry Determination of pymetrozine residues in food for export by liquid chromatography-mass spectrometry/mass spectrometry Mass Spectrometry of Cyproheptadine No peak in gas chromatography mass spectrometry GC mass spectrometry does not produce peaks from time to time MS mass 18 mass spectrometry Parameters for Chromatography and Mass Spectrometry MS co-elution LC-MS co-elution Liquid chromatography + peak extraction Liquid chromatography peaks within a few minutes at the earliest Liquid chromatography peaks in 70 minutes Gas source for mass spectrometry mass spectrum peak MS effluent Liquid chromatography peaks in one minute Quantification by mass spectrometry LC peaks prematurely MS co-elution Monitoring of Residues in Exported Foods of Animal Origin Mass Spectrometry Liquid Chromatography Peak Relative Quantification and Absolute Quantification by Mass Spectrometry Absolute quantitation by mass spectrometry Foods of Animal Origin Liquid Chromatography LC outlet ring Mass Spectrometry Internal Quantification Mass Spectrometry + Determination + Quantity liquid measurable substance Absolute quantitation by mass spectrometry Mass spectrometry operation Mass spectrometry + semi-quantitative Absolute Quantification and Relative Quantification by Mass Spectrometry Quantitative mass spectrometry Mass Spectrum 41 Peak Mass Spectrometry Relative and Absolute Quantification Chromatographic mass fraction as5148 Absolute and Relative Quantification by Mass Spectrometry Relative and Absolute Quantification by Mass Spectrometry Chromatography of animal origin Mass Spectrometry Relative Quantification Absolute Quantification Negative peaks appear in the chromatogram Mobile phase for mass spectrometry Can liquid chromatography mass spectrometry detect inorganic substances? Liquid chromatography mass spectrometry APCI source Mass spectrum animation Mass Spectrometry Method EI Source Compounds with no peaks in the mass spectrum Liquid Chromatography Mass Spectrometry Competition Scoring Mass spectrometry power supply stability test

Introduction

Analysis of the core content of the standard

Technical elements	Clenbuterol	Cyproheptadine
Molecular formula	C₉H₁₀Cl₃N₃	C₂₁H₂₂ClN
CAS number	4205-91-8	41354-29-4
Limit of quantitation (LOQ)	5.0 μg/kg
Characteristic ion pairs (m/z)	229.6/213.0 229.6/187.1	288.2/215.1 288.2/191.1

Method technology evolution

This standard uses liquid chromatography-tandem mass spectrometry to replace the traditional ELISA method, which significantly improves the detection specificity:

Pretreatment optimization: Acetonitrile extraction combined with mixed-mode SPE column cleanup, the recovery rate is increased to 70%-102%
Chromatographic separation: T3 chromatographic column (100mm×2.1mm,1.8μm) to achieve baseline separation, retention time of clenbuterol is 3.25min
Mass spectrometry conditions: In ESI+ mode, the collision energies were optimized to 30eV (clenbuterol) and 23eV (cyproheptadine)

Key operating points

Sample preparation specifications

Muscle/liver: homogenize and store at -18℃ to avoid repeated freezing and thawing
Fat samples: thaw in a 45-50℃ water bath and then homogenize
Egg products: homogenize the whole egg after removing the eggshell

Quality control requirements

Relative ion abundance ratio	Allow deviation ≤±25%
Retention time	Deviation ≤±2.5%

Implementation suggestions

Key points for method validation

Linear range: 0-100ng/mL (r≥0.99)
Matrix effect assessment: verified by standard addition method
Perform blank spike experiments regularly (5μg/kg level is recommended)

Solutions to common problems

Decrease in sensitivity: Check ion source contamination and optimize sheath gas (241.3kPa) and auxiliary gas (55.1kPa) pressures

Peak tailing: Change the formic acid concentration in the mobile phase (0.2%) and maintain the column temperature at 30°C

More samples: NB/T 47013.2-2015 DL/T 368-2010 JC/T 2453-2018

Sample only — not a preview of SN/T 5148-2019

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