SN/T 5446-2022 in English
VALIDDetermination 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
$175.00
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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