A method for the identification of relevant impurities in illegal o-chlorophenyl cyclopentyl ketone drug was developed. Identification of impurities could help regulation of this illegal drug and allow the sources of samples of the drug to be identified. An efficient and effective method for qualitatively analyzing samples using high performance liquid chromatography-hybrid ion trap/time-of-flight mass spectrometry (HPLC-IT/TOF MS) was developed. The o-chlorophenyl cyclopentyl ketone fragmentation pathway during HPLC-MSn was determined by analyzing a standard by HPLC-IT/TOF MS. The optimized HPLC-IT/TOF MS method allowed two impurities in o-chlorophenyl cyclopentyl ketone samples to be identified. According to the exact mass data of MSn and the element composition analysis, two impurities were identified as o-chlorobenzoic acid anhydride and 1,2-di-o-chlorobenzoylcyclopentene. The synthetic route of the o-chlorophenyl cyclopentyl ketone samples was proposed by analysis of these impurities. The established method made it easy to identify impurities and find the source of this illegal drug. A method for the preparation an o-chlorophenyl cyclopentyl ketone reference standard from actual samples using preparative HPLC was also developed. The mobile phase was methanol-water (85:15, v/v) and flow rate was 8 mL/min. The purity of the obtained standards, determined by analytical HPLC, was 99.53%. This method is simple, efficient, and can be used for the preparation of other illegal drugs.

中文翻译：

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高效液相色谱-混合离子阱/飞行时间质谱鉴定邻氯苯基环戊基酮样品中的杂质并制备邻氯苯基环戊基酮标准品

提出了一种鉴别非法邻氯苯基环戊基酮药物中相关杂质的方法。杂质的识别可以帮助管制这种非法药物，并可以识别药物样品的来源。建立了一种高效，高效的定性分析样品的方法，该方法采用高效液相色谱-混合离子阱/飞行时间质谱（HPLC-IT / TOF MS）。通过HPLC-IT / TOF MS分析标准品，可以确定HPLC-MSn中邻氯苯基环戊基酮的裂解途径。通过优化的HPLC-IT / TOF MS方法，可以鉴定邻氯苯基环戊基酮样品中的两种杂质。根据MSn的准确质量数据和元素组成分析，确定了两种杂质：邻氯苯甲酸酐和1，2-二邻氯苯甲酰基环戊烯。通过对这些杂质的分析，提出了邻氯苯基环戊基酮样品的合成路线。既定的方法使人们很容易识别杂质并找到这种非法药物的来源。还开发了使用制备型HPLC从实际样品中制备邻氯苯基环戊基酮参考标准品的方法。流动相为甲醇-水（85:15，v / v），流速为8 mL / min。通过分析型HPLC确定所获得的标准品的纯度为99.53％。该方法简单，有效，可用于制备其他非法药物。既定的方法使人们很容易识别杂质并找到这种非法药物的来源。还开发了使用制备型HPLC从实际样品中制备邻氯苯基环戊基酮参考标准品的方法。流动相为甲醇-水（85:15，v / v），流速为8 mL / min。通过分析型HPLC确定所获得的标准品的纯度为99.53％。该方法简单，有效，可用于制备其他非法药物。既定的方法使鉴定杂质和发现这种非法药物的来源变得容易。还开发了使用制备型HPLC从实际样品中制备邻氯苯基环戊基酮参考标准品的方法。流动相为甲醇-水（85:15，v / v），流速为8 mL / min。通过分析型HPLC确定所获得的标准品的纯度为99.53％。该方法简单，有效，可用于制备其他非法药物。