GA/T 208-2019 in English
VALIDForensic sciences—Examination methods for phosphide in biological samples—HSGC and HSGC-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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本标准规定了生物检材（血、尿、肝、肾、胃及胃内容等）中磷化氢的顶空气相色谱（HSGC）定量检验、顶空气相色谱-质谱（HSGC-MS）定性定量检验方法。
本标准适用于生物检材中磷化氢的定性分析和定量分析。其他可疑样品中磷化氢的定性分析和定量分析可参照使用。
Introduction
Core changes in the standard revision
| Comparison dimensions | GA/T 208-1999 | GA/T ××××-×××× | Technical significance |
|---|---|---|---|
| Detection method | AgDDC method + mercuric bromide test paper method | HSGC/HSGC-MS | Sensitivity increased by 10^3 times |
| Detection limit | Undefined | 500ng/mL(g) | Quantitative detection capability |
| Metabolite detection | Phosphine only | Phosphine + phosphorous acid metabolites | Extended detection window |
Technical principle innovation
The new standard adopts a dual reduction mechanism: hydrogen is generated by the reaction of zinc powder and sulfuric acid, and the phosphorous acid produced by metabolism in the body is reduced to phosphine (see Appendix B for the reaction formula), and then gas-liquid separation is achieved through a headspace sampler. Compared with traditional methods:
- Sensitivity: FPD-P detector has a characteristic response of 10^-12g to phosphorus
- Specificity: The deviation of the abundance ratio of mass spectrometry characteristic ions 34 (PH+) and 31 (P+) is ≤15%
Key operating points
Typical case operation flow
Liver tissue detection in a poisoning case:
- Weigh 1.0g of sample and add it to a 10mL headspace bottle containing zinc powder
- Add 2mL of water + 0.5mL of 20% sulfuric acid solution
- Equilibrate at 45℃ for 10min before GC-MS analysis
- Confirm the positive result by the ratio of PH+ (m/z34) to P+ (m/z31) ions
Implementation Suggestions
| Steps | Precautions | Quality Control Requirements |
|---|---|---|
| Sample pretreatment | Solid samples must be fully homogenized | Parallel sample RD≤20% |
| Instrument calibration | Perform FPD linearity verification every week | R²≥0.995 |
| Data review | Characteristic ion abundance ratio must be checked | Consistent with the deviation range in Table 1 |
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