GA/T 1602-2019 in English
VALIDForensic sciences—Examination methods for diazepam and its metabolites in biological samples—LC and LC-MS
- Issued on:2019-10-01
- 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）中地西泮及其代谢物（去甲西泮、去甲羟基西泮、去甲羟基西泮葡萄糖醛酸苷、羟基西泮葡萄糖醛酸苷）的高效液相色谱（HPLC）及液相色谱-串联质谱（LC-MS/MS）定性定量检验方法。
本标准适用于法庭科学生物检材中地西泮及其代谢物（去甲西泮、去甲羟基西泮、去甲羟基西泮葡萄糖醛酸苷、羟基西泮葡萄糖醛酸苷）的定性分析和定量分析。其他可疑样品中地西泮及其代谢物的定性分析和定量分析可参照使用。
Introduction
Analysis of the core content of the standard
This standard specifies the technical specifications for the detection of diazepam and its five metabolites in biological samples by high performance liquid chromatography and liquid chromatography-tandem mass spectrometry. Among them, glucuronide-bound metabolites are innovatively included in the detection scope, expanding the coverage dimension of traditional detection methods.
Comparison of key technical parameters
| Test items | HPLC conditions | LC-MS/MS conditions | Detection limit (ng/mL) |
|---|---|---|---|
| Diazepam | 250mm C18 column, 250nm detection | MRM mode, 285>154 ion pair | 1 |
| N/A | MRM mode, 463>287 ion pair | 5 |
Key points for implementation of the standard
Application of typical cases
In a drug-related case, when this standard was used to test the liver tissue of the deceased, 0.8μg/g of nordiazepam metabolites were detected by LC-MS/MS after purification by solid phase extraction column. Key operation points include:
- Methanol/ammonia/water eluents were strictly prepared in a ratio of 5:2:93
- Solid phase extraction flow rate was controlled to ≤0.5mL/min
- At least two pairs of qualifier ions should be monitored during mass spectrometry analysis
Method validation data
Standard validation data showed that within the linear range of 1-100ng/mL, the recovery of diazepam reached 85-110%, and the intra-day precision RSD was <8%. It is particularly important to note that hydroxy metabolites are easily hydrolyzed under acidic conditions, and it is recommended to complete the test within 24 hours after sample extraction.
Technology Evolution Analysis
Compared with the old method, the main improvements of this standard are:
- LC-MS/MS is added as a confirmation method
- Detection limit is reduced by 5-10 times
- Inclusion of glucuronide metabolite detection
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