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手性 HPLC-DAD 拆分缴获片剂中顺式 CPP 对映异构体。

Separation of positional CPP isomers by chiral HPLC-DAD of seized tablets.

机构信息

Institute of Forensic Medicine Münster, Röntgenstr. 23, 48149, Münster, Germany.

出版信息

Int J Legal Med. 2011 Jan;125(1):95-9. doi: 10.1007/s00414-010-0422-z. Epub 2010 Feb 17.

Abstract

Meta-chlorophenylpiperazine, one of the synthetic piperazine-derived designer drugs, is to date controlled as an illicit substance in five European member states. Depending on the position of the chlorine atom, different positional isomers of CPP (ortho-, meta- and para-) are possible. Therefore, there is a need to develop an analytical method for the separation and identification of the three 1-chlorophenylpiperazines in tablets containing CPP. In this work, the position isomers o-, m- and p-CPP were separated by liquid chromatography (HPLC) on a reversed-phase chiral column. Different mobile phase compositions and pH ranges were systematically studied to find optimum chromatographic conditions. Best results were achieved with isocratic mobile phase of triethyl amine buffer and methanol (V/V = 70/30) at pH 9 with a flow rate of 0.8 ml/min. The method was validated in terms of selectivity, linearity, limit of detection and quantification and precision. At last, the developed method was successfully applied on seized ecstasy tablets.

摘要

间氯苯哌嗪,一种合成苯丙胺类兴奋剂,目前在五个欧洲成员国被列为非法物质。根据氯原子的位置,CPP(邻位、间位和对位)可能存在不同的位置异构体。因此,有必要开发一种分析方法,用于分离和鉴定含有 CPP 的片剂中的三种 1-氯苯哌嗪。在这项工作中,间位异构体 o-、m-和 p-CPP 通过反相手性柱的液相色谱(HPLC)进行了分离。系统研究了不同的流动相组成和 pH 范围,以找到最佳的色谱条件。在 pH 9 时,使用三乙胺缓冲液和甲醇(V/V=70/30)的等度流动相,流速为 0.8 ml/min,可获得最佳结果。该方法在选择性、线性、检测限和定量限以及精密度方面进行了验证。最后,该方法成功应用于缴获的摇头丸片剂。

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