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lc-ms/ms method introduction analysis quechers pretreatment method ultrasonic double extraction acetonitrile homogenization extraction purification technology psa+c18 oxine copper standard technical framework technical circulating fluidized bed boilers part5 metal dentate gaskets comprehensive evaluation index system
SN/T 5446-2022 in English

SN/T 5446-2022 in English

VALID

Determination of residue of oxine copper in plant-origin foodstuffs 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): $180.00
$175.00
Standard No: SN/T 5446-2022
Document status: VALID
Title in English: Determination of residue of oxine copper in plant-origin foodstuffs for export - LC-MS/MS method
Title in Chinese: 出口植物源性食品中喹啉铜残留量的测定 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: lc-ms/ms method introduction analysis
quechers pretreatment method
ultrasonic double extraction acetonitrile homogenization extraction purification technology psa+c18
oxine copper
standard technical framework technical
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Introduction

Analysis of standard technical framework

Technical elements Requirements of this standard Comparison of conventional methods
Extraction method 1% acetic acid ultrasonic double extraction Acetonitrile homogenization extraction
Purification technology PSA+C18 composite purification Single adsorbent purification
Detection limit 0.1mg/kg 0.5mg/kg
Chromatographic conditions ODS-4 column + gradient elution C18 isocratic elution

Key technical points

1. Pretreatment optimization

Using ultrasonic cleaner and 1% acetic acid solution for double extraction, the extraction efficiency of copper complex in complex matrix samples such as tomatoes reached more than 92%. The composite purification system of PSA and C18 can effectively remove pigments (purification rate> 85%) and lipid interferences.

2. Instrument parameter settings

The mass spectrometer uses 146.07/118.05 as the quantitative ion pair, and the signal-to-noise ratio is best when the collision energy is 22.28eV. The acetonitrile ratio is increased to 30% at 5 minutes in the chromatographic gradient program, which can shorten the analysis time to 10 minutes/sample.


Implementation suggestions

1. Key points of quality control

  • Standard solutions must be prepared and used immediately (valid for 3 weeks)
  • Matrix matching standard curves must be made for each batch of samples
  • Retention time deviations must be controlled within ±2.5%

2. Abnormal handling plan

When the recovery rate exceeds the range of 80-120%, check whether the centrifuge speed reaches 12000r/min, or replace the PSA adsorbent batch.


Standard Evolution Analysis

This method has the following improvements compared to GB 23200.113-2018: ①The limit of quantification is reduced by 80% ②The applicability of matrices such as pecans is increased ③Formic acid is used to improve the mobile phase to enhance the peak shape. It may develop towards the QuEChERS pretreatment method in the future.

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