SN/T 5169-2019 in English
VALIDDetermination of methenolone in animal- -origin foodstuffs for export-LC-MS /MS method
- Issued on:2019-10-25
- Implemented on:2020-05-01
- File Format:PDF
- Delivery:Via email within 5 business days
$262.00
Introduction
Technical background and significance of the standard
Methenolone is a synthetic steroid drug. Illegal use in animal breeding may lead to food residue risks. This standard, which is formulated for the detection method of liquid chromatography-mass spectrometry/mass spectrometry for exported animal-derived foods, fills the gap in the detection standard of this type of substance in my country. The detection limit reaches 0.5 μg/kg, meeting the technical regulations of major trading bodies such as the European Union.
Core Technology Innovation of the Method
| Technical Links | Traditional Methods | Improvements of This Standard |
|---|---|---|
| Pretreatment | Single Organic Solvent Extraction | Formic Acid-Acetonitrile Co-extraction Combined with Enzymatic Hydrolysis (β-Glucuronidase) |
| Purification Method | Traditional SPE Column Purification | PRiME HLB Solid Phase Extraction and Dispersive Solid Phase Extraction (PSA+C18) Dual Mode Selection |
| Detection Sensitivity | 1-5 μg/kg | 0.5 μg/kg (pork matrix) |
Analysis of key operating points
Optimization of sample pretreatment differences
Different treatments were used for different matrices:
• Meat products: After enzymatic hydrolysis, only 1% formic acid and acetonitrile were required for extraction
• Dairy products: Additional addition of anhydrous sodium sulfate for dehydration increased the recovery rate by 12.7%
Case of mass spectrometry parameter optimization
The optimal CE value was determined by collision energy gradient experiment:
The signal-to-noise ratio of the quantitative ion pair 303.1→83.0 of Primobolan reached its peak at 23 eV, which increased the detection sensitivity by 1.8 times compared with the conventional 20 eV
Implementation recommendations and quality control points
- Internal standard selection: Use methyltestosterone-d3 instead of structural analogs to correct for the matrix effect (ME≤15%)
- Method validation: Cross-validation of different animal-derived matrices is required, and special attention should be paid to ion suppression in milk matrices
- Equipment maintenance: The electrospray ion source needs to be capillary voltage calibrated weekly, and maintenance is required if the deviation exceeds ±200V
Technology development prospects
With the popularization of high-resolution mass spectrometry technology, the following can be expanded in the future:
1) Non-target screening strategy
2) Combined detection of metabolites (such as 17-hydroxymethenolone)
3) Compatibility study of automated pretreatment equipment
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