类苯哌嗪类化合物的分析

H. Inoue, Y. Iwata, T. Kanamori, H. Miyaguchi, K. Tsujikawa, K. Kuwayama, H. Tsutsumi, M. Katagi, H. Tsuchihashi, T. Kishi
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引用次数: 12

摘要

对2003年日本新管制的1-苄基哌嗪(BZP)和1-(3-三氟甲基苯基)哌嗪及其类似物进行分析。采用显色法、薄层色谱法、红外光谱法、气相色谱/质谱法和液相色谱/质谱法对样品进行了分析。类bzp化合物对西蒙试剂的敏感性低于苯丙胺类兴奋剂。使用基于Simon测试(X-Checker®)的现场筛选试剂盒,BZP显示的结果与甲基苯丙胺几乎相同。对于薄层色谱,溶剂体系,甲醇- 25%的水氨(100:1.5)是最好的。碘铂酸盐是检测BZP最敏感的试剂。红外光谱显示出足够的差异,可以进行鉴别。在峰形、分离度和稳定性方面(使用J&W DB-5MS柱),三甲基硅基化是对bzp类化合物进行GC/MS分析的最合适选择。在LC/MS分析中,使用Waters Symmetry Shield C18柱梯度洗脱(10 mM甲酸和乙腈)实现了除1-(2-氟苯基)哌嗪和1-(4-氟苯基)哌嗪外的异构体的区分。LC/MS筛选时推荐锥面电压为30v。这些资料将有助于鉴定没收的粉末、液体或片剂中的哌嗪。
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Analysis of Benzylpiperazine-like Compounds
1-Benzylpiperazine (BZP) and 1-(3-trifluoromethylphenyl)piperazine, newly controlled as narcotics in Japan on 2003, and their analogues were analyzed. The analytical data with color test, thin layer chromatography (TLC), infrared spectroscopy (IR), gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/mass spectrometry (LC/MS) are presented.   The BZP-like compounds were less sensitive to Simon's reagent than amphetamine type stimulants on spot plates. Using on-site screening kit based on Simon's test (X-Checker®), BZP indicated almost the same result as methamphetamine. For TLC, the solvent system, methanol −25% aqueous ammonia (100 : 1.5), was the best among the systems examined. Iodoplatinate reagent was the most sensitive one to detect BZP. The IR spectra showed sufficient differences to make identification. Trimethylsilylation was the most appropriate choice for the GC/MS analysis of BZP-like compounds in terms of the peak shapes, separation and stability (using a J&W DB-5MS column). In LC/MS analysis, the gradient elution (10 mM formic acid and acetonitrile) using a Waters Symmetry Shield C18 column achieved discrimination of isomers except for 1-(2-fluorophenyl)piperazine and 1-(4-fluorophenyl)piperazine. The cone voltage of 30 V was recommended for the LC/MS screening. The information would be useful for identification of piperazines in confiscated powders, liquids or tablets.
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