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地西泮衍生化和 GC-MS 分析会产生错误的去甲西泮和奥沙西泮结果。

Demoxepam Derivatization and GC-MS Analysis Produces Erroneous Nordiazepam and Oxazepam Results.

机构信息

New York State Police Forensic Investigation Center, 1220 Washington Ave, Bldg 30, Albany, NY, USA.

出版信息

J Anal Toxicol. 2019 Jun 1;43(5):406-410. doi: 10.1093/jat/bkz006.

DOI:10.1093/jat/bkz006
PMID:30796822
Abstract

Demoxepam, when derivatized by silylation and analyzed using gas chromatography-mass spectrometry (GC-MS), produces artifacts which are falsely identified as nordiazepam and oxazepam. Demoxepam was analyzed unextracted at various concentrations, using different derivatization procedures, and on different GC-MS systems. Oxazepam and nordiazepam were consistently identified in neat demoxepam samples, despite the changing variables. Under certain conditions, oxazepam was identified as low as 50 ng/mL derivatized demoxepam, and nordiazepam identified as low as 500 ng/mL derivatized demoxepam. The analysis of underivatized demoxepam resulted in nordiazepam detection at levels ≥2,500 ng/mL, whereas oxazepam was not detectable at or below 10,000 ng/mL demoxepam. Isolating the derivatization procedures and GC-MS analyses demonstrates that these processes are responsible for any degradation or rearrangement reactions which are taking place. Laboratories which follow similar procedures for benzodiazepine confirmations should consider these findings when interpreting analytical data from chlordiazepoxide cases.

摘要

地西泮经硅烷化衍生化后,用气相色谱-质谱联用仪(GC-MS)分析,会产生假象,被错误地鉴定为去甲西泮和奥沙西泮。地西泮未经提取,在不同浓度下,使用不同的衍生化程序和不同的 GC-MS 系统进行分析。在未衍生的地西泮样品中,奥沙西泮和去甲西泮一直被识别出来,尽管变量在不断变化。在某些条件下,衍生化的地西泮中低至 50ng/mL 的奥沙西泮可被识别,衍生化的地西泮中低至 500ng/mL 的去甲西泮可被识别。未衍生化的地西泮分析导致去甲西泮的检测水平≥2500ng/mL,而奥沙西泮在 10000ng/mL 或以下的地西泮中无法检测到。分离衍生化程序和 GC-MS 分析表明,这些过程是造成任何降解或重排反应的原因。遵循类似苯二氮䓬确证程序的实验室在解释氯氮䓬案例的分析数据时,应考虑这些发现。

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