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internal standard method single solvent purification method scx cation exchange column c18 lc-ms/ms method introduction analysis method comparison method chemical fibre filature machine scopethis standard 43879-2024 service-oriented manufacturing mercury displacement method
SN/T 5437-2022 in English

SN/T 5437-2022 in English

VALID

Determination of diphenhydramine residue in foodstuffs of animal origin for export - LC-MS/MS method

  • Issued on:2022-03-14
  • Implemented on:2022-10-01
  • File Format:PDF
  • Delivery:Via email within 1~3 business days
Price(USD): $220.00
$214.00
Standard No: SN/T 5437-2022
Document status: VALID
Title in English: Determination of diphenhydramine residue in foodstuffs of animal origin for export - LC-MS/MS method
Title in Chinese: 出口动物源食品中苯海拉明残留量的测定 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: 2022-03-14
Implemented on: 2022-10-01
Professional Classification: SN-Import&Export Inspection
Related Keywords: internal standard method
single solvent purification method scx cation exchange column c18
lc-ms/ms method introduction analysis
method comparison
method
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Introduction

Analysis of standard technical framework

Technical elements Characteristics of this method Comparison with conventional methods
Extraction solvent 1% trichloroacetic acid-acetonitrile (3:7) Acetonitrile or methanol single solvent
Purification method SCX cation exchange column C18 or HLB column
Detector Triple quadrupole MRM mode Single quadrupole SIM mode

Key technological breakthroughs

The standard innovatively uses liquid chromatography-mass spectrometry/mass spectrometer combined with isotope internal standard method (diphenhydramine-D3), and by optimizing the extraction solvent ratio and SCX column purification process, the quantitative limit of complex matrices such as pork is reduced to 5 μg/kg, and the milk matrix is even reduced to 1 μg/kg.


Operational points

Typical application case

A suspected positive sample (detection value 8.2 μg/kg) was found in the test of a beef export enterprise. After the confirmation process specified in the standard (retention time deviation <2.5%, ion abundance ratio meets the requirements of Appendix B), it was finally confirmed that the diphenhydramine residue came from the abuse of antihistamines in the breeding process.


Recommendations for the implementation of the standard

  1. Laboratories need to regularly verify the nebulizer gas flow rate (recommended 8 L/min) and collision energy (256→167.1 channel maintained at 60 eV) of the electrospray ion source
  2. For high-fat samples (such as pig intestines), it is recommended to add a n-hexane defatting step
  3. The standard working solution should be prepared and used immediately to avoid degradation of the formic acid-acetonitrile system

Technology evolution analysis

Compared with the 2008 version of the Ministry of Agriculture standard, the progress of this standard is reflected in: ①Introducing isotope internal standards to compensate for matrix effects ②Using 1.8 μm ultra-high efficiency chromatographic columns to increase throughput ③Adding verification data for special matrices such as pig kidneys. In the future, it can develop in the direction of multi-residue joint testing.

Sample only — not a preview of SN/T 5437-2022
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