GA/T 1627-2019 in English
VALIDForensic sciences—Examination methods for four phenoxyacid herbicides including 2,4-D in biological samples—GC and GC-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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本标准规定了法庭科学生物检材（血、尿、肝、肾、胃及胃内容等）中2,4-D (2,4-二氯苯氧乙酸、2,4-滴）、2,4-DP［2-（2,4-二氯苯氧）-丙酸,又称2,4-滴丙酸］、MCPA（4-氯-2-甲基-苯氧乙酸,又称2甲4氯）和MCPP［2-（4-氯-2-甲基-苯氧）-丙酸,又称2甲4氯苯氧丙酸］4种苯氧羧酸类除草剂的气相色谱（GC）定量检验方法和气相色谱-质谱（GC-MS）定性定量检验方法。
本标准适用于法庭科学生物检材中2,4-D、2,4-DP、MCPP和MCPA的定性分析和定量分析。其他可疑样品中2,4-D、2,4-DP、MCPP和MCPA的定性分析和定量分析可参照使用。
Introduction
Analysis of Standard Technical Framework
| Technical Dimension | GC Method | GC-MS Method |
|---|---|---|
| Detector Type | ECD Electron Capture | EI Mass Spectrometry |
| Derivatization Reagent | Dichloropropanol | n-Butanol |
| Detection Limit (Blood Sample) | 8-40ng/mL | 26-74ng/mL |
| Qualitative Basis | Retention time | Characteristic ion fragments (≥3) |
Key operation points
Derivatization control: n-Butyl derivatization requires room temperature reaction for 30 minutes, dichloropropyl derivatization requires 80℃ water bath for 90 minutes, and sodium bicarbonate solution is required for purification after the reaction.
Mass spectrometry characteristic ions: Characteristic fragments such as 2,4-D (m/z185) and MCPP (m/z169) must meet the abundance ratio deviation of ≤20%.
Technology Evolution Background
This standard targets herbicides such as 2,4-D, which are common in agricultural poisoning cases. By optimizing the GDX401 solid phase extraction and derivatization technology, the detection limit of plant samples is reduced to 16ng/g, which is 40% higher than the efficiency of traditional liquid-liquid extraction.
Implementation Suggestions
- Blood samples should preferably use solid phase extraction (recovery rate > 98%)
- GC-MS full scan and SIM mode are recommended for difficult samples
- Regularly verify the purity of the derivatization reagent (sulfuric acid needs to be ≥ 98%)
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