Impurity profiling of methamphetamine hydrochloride drugs seized in the Philippines

Impurity profiling of methamphetamine hydrochloride drugs seized in the Philippines
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DOI:
10.1016/j.forsciint.2004.03.002
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发表时间:
2004-08-11
影响因子:
2.2
通讯作者:
Dumlao, MC
Dumlao, MC
中科院分区:
医学3区
文献类型:
--
作者:
Dayrit, FA;Dumlao, MC

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盐酸甲苯胺非他明是菲律宾使用最广泛的非法药物之一。在这项研究中,我们描述了应用聚类分析的痕量杂质的分析中查获的甲基苯丙胺药物样品的概况。将30毫克均质化的药物样品溶解在1 mL pH 10.5缓冲溶液中,并用含有三种内标物的乙酸乙酯萃取。使用气相色谱-质谱法(GC-MS)鉴定痕量杂质,并通过气相色谱-火焰离子化检测器(GC-FID)进行定量。根据先前报道的方法,从GC-FID色谱图中选择30个杂质峰。峰面积和保留时间参考内标物。然后将所选峰的峰面积分组用于聚类分析。为了检查聚类的一致性,使用40和50个杂质峰进行了两次进一步的聚类分析。在30至40个杂质峰中观察到聚类变化,而使用40和50个杂质峰的分析得到了相似的结果。因此,对于本研究中使用的缉获药物样品,使用至少40个杂质峰的聚类分析比仅使用30个峰的聚类分析显示出更好的聚类一致性,确定了10个杂质峰,其中4个是首次在甲基苯丙胺药物样品中确定的。它们是对溴甲苯、N-苄基苯丙胺、N-乙基苯丙胺和N-乙基甲基苯丙胺。苯基-2-丙酮(P2P)、N,N-二甲基苯丙胺和N-甲酰基苯丙胺的存在表明这些个案样品是使用Leuckart方法合成的。(C)2004爱思唯尔爱尔兰有限公司保留所有权利。
Methaniphetamine hydrochloride is one of the most widely used illicit drugs in the Philippines. In this study, we describe the application of cluster analysis of trace impurities in the profiling of the seized methamphetamine drug samples. Thirty milligrams of a homogenized drug sample were dissolved in I mL of pH 10.5 buffer solution and extracted with ethyl acetate containing three internal standards. The trace impurities were identified using gas chromatography-mass spectrometry (GC-MS) and quantified by gas chromatography with a flame ionization detector (GC-FID). Following previously reported methodologies, 30 impurity peaks were selected from the GC-FID chromatograms. The peak areas and retention times were referenced to the internal standards. The peak areas of the selected peaks were then grouped for cluster analysis. In order to check for consistency of clustering, two further cluster analyses were performed using 40 and 50 impurity peaks. Changes in clustering were observed in going from 30 to 40 impurity peaks, while analyses using 40 and 50 impurity peaks gave similar results. Thus, for the seized drug samples used in this study, cluster analysis using at least 40 impurity peaks showed better consistency of clustering as compared to analysis using 30 peaks only.Ten of the impurity peaks were identified, of which four were identified for the first time in methamphetamine drug samples. These are p-bromotoulene, N-benzyl amphetamine, N-ethyl amphetamine, and N-ethyl methamphetamine. The presence of phenyl-2-propanone (P2P), N,N-dimethyl amphetamine, and N-formyl amphetamine is indicative that these casework samples were synthesized using the Leuckart method. (C) 2004 Elsevier Ireland Ltd. All rights reserved.