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用于药物筛查和确证的全二维气相色谱-飞行时间质谱联用技术(GC×GC-TOFMS)

Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GC x GC-TOFMS) for drug screening and confirmation.

作者信息

Song Shin Miin, Marriott Philip, Kotsos Alex, Drummer Olaf H, Wynne Paul

机构信息

Department of Applied Chemistry, Australian Centre for Research on Separation Science, Rmit University, Building 3, Bowen St., 124 Latrobe St., GPO Box 2476 V, Melbourne, Vic. 3001.

出版信息

Forensic Sci Int. 2004 Jul 16;143(2-3):87-101. doi: 10.1016/j.forsciint.2004.02.042.

Abstract

Comprehensive two-dimensional gas chromatography (GC x GC) is applied to analysis of drug standard mixtures containing 78 drugs of interest in forensic samples. For this study, underivatised drugs were employed. While several of the drugs were not detected at the low concentrations employed in the samples, most could be satisfactorily assigned their first and second dimension retentions in the GC x GC retention plane. For this study, time-of-flight mass spectrometry (TOFMS) detection was used. The enhanced separation possible in GC x GC is demonstrated, and typical linearity and apparatus precision are shown for tramadol, diazepam, olanzapine and desipramine using selected qualifier ions. Mass spectral library search quality for the detection of drugs in a selection of authentic forensic cases, along with retention position in the 2D retention plane, is used to support positive identification of the presence of the drugs. The analysis of 'difficult' drugs paracetamol and phenytoin is shown to produce anomalous chromatographic peak shape in the 2D plane, whereas most drugs gave acceptable peak shapes. The GC x GC technique was applied to screening drugs in forensic samples, with either flame ionisation (FID) or TOFMS detection, and compared favourably with conventional single column GC-MS analysis when tested for diazepam in an authentic forensic study.

摘要

全二维气相色谱法(GC×GC)被应用于分析法医样本中含78种目标药物的药物标准混合物。在本研究中,使用了未衍生化的药物。虽然在样本所采用的低浓度下有几种药物未被检测到,但大多数药物在GC×GC保留平面中都能令人满意地确定其第一维和第二维保留时间。在本研究中,使用了飞行时间质谱(TOFMS)检测。展示了GC×GC中可能实现的增强分离效果,并使用选定的定性离子显示了曲马多、地西泮、奥氮平和地昔帕明的典型线性和仪器精密度。在一系列真实法医案例中检测药物时的质谱库检索质量,以及在二维保留平面中的保留位置,被用于支持对药物存在的阳性鉴定。对“难分析”的药物对乙酰氨基酚和苯妥英的分析显示,在二维平面中会产生异常的色谱峰形,而大多数药物的峰形是可接受的。GC×GC技术被应用于法医样本中的药物筛查,采用火焰离子化(FID)或TOFMS检测,在一项真实法医研究中针对地西泮进行测试时,与传统的单柱GC-MS分析相比具有优势。

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