GA/T 1618-2019 in English
VALIDForensic sciences—Examination methods for methadone in biological samples—LC-MS
- Issued on:2019-10-14
- Implemented on:2019-12-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
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Introduction
Analysis of the core content of the standard
This standard establishes a complete technical framework for the detection of methadone in biological samples using liquid chromatography-mass spectrometry. Its innovation is reflected in:
| Technical dimensions | Ion trap mass spectrometry configuration | Triple quadrupole mass spectrometry configuration |
|---|---|---|
| Chromatographic column specifications | C18 column (2.1×150mm,3.5µm) | UPLC BEH C18 column (2.1×50mm,1.7µm) |
| Analysis time | 19 minutes/sample | 3.5 minutes/sample |
| Characteristic ion pairs | 310.2→264.9 | 310.31→105.04/265.18 |
Key technical points
Sample pretreatment specifications
The solid phase extraction process uses a mixed cation exchange column (MCX), and selective adsorption is achieved by pH adjustment:
- Methadone is protonated under acidic conditions (pH<3)
- Elution with aminated acetonitrile (5% ammonia water) ensures a recovery rate of >85%
- The concentration temperature is strictly controlled at 50±2℃
Mass spectrometry parameter optimization
Different settings are given for different mass spectrometry types:
- Ion trap mode: secondary full scan m/z 264.9 as quantitative ion
- Triple quadrupole mode: MRM monitoring of two pairs of ions (310→105/265)
- Collision energy optimization range24-35eV
Implementation and application guide
Typical case analysis
In a drug-related death case, this standard was used to detect liver tissue:
- The detected concentration was 4.2µg/g, exceeding the lethal threshold
- The mass spectrum shows characteristic ions 264.9/310.2
- Relative abundance ratio deviation <15%
Common Problems
| Problem phenomenon | Possible cause | Solution |
|---|---|---|
| Low recovery rate | Insufficient activation of SPE column | Increase methanol activation volume to 2mL |
| Obvious matrix effect | Incomplete sample purification | Add isotope internal standard d3-methadone |
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