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Impurity profiling of methamphetamine hydrochloride drugs seized in the Philippines.

机译:在菲律宾缉获的盐酸甲基苯丙胺药物的杂质分析。

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Methamphetamine 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 1mL 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-bromotoluene, 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.
机译:盐酸甲基苯丙胺是菲律宾使用最广泛的非法药物之一。在这项研究中,我们描述了痕量杂质的聚类分析在缉获的甲基苯丙胺药物样品谱图中的应用。将三十毫克均质的药物样品溶于1mL pH 10.5的缓冲溶液中,并用含三种内标的乙酸乙酯萃取。使用气相色谱-质谱法(GC-MS)鉴定痕量杂质,并使用火焰离子化检测器(GC-FID)通过气相色谱法定量。按照先前报道的方法,从GC-FID色谱图中选择了30个杂质峰。峰面积和保留时间参考内标。然后将所选峰的峰面积分组以进行聚类分析。为了检查聚类的一致性,使用40和50个杂质峰进行了另外两个聚类分析。从30个杂质峰到40个杂质峰观察到了聚类的变化,而使用40个杂质峰和50个杂质峰的分析得出了相似的结果。因此,对于本研究中使用的缉获药物样品,与仅使用30个峰进行分析相比,使用至少40个杂质峰进行聚类分析显示出更好的聚类一致性。鉴定出了十个杂质峰,其中四个在甲基苯丙胺药物样品中首次被鉴定。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案例样品是使用Leuckart方法合成的。

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