氯胺酮杂质的超高效液相色谱-质谱法分析及其关联性判别应用

Impurity Profiling of Ketamine and Its Applications on Correlation Analysis

分别使用超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF MS)和超高效液相色谱-三重四极杆质谱(UPLC-QqQ-MS)联用技术,分离、筛选并测定氯胺酮中的17种杂质。首先,使用UPLC-Q-TOF MS检测并筛选出氯胺酮中的17种特征杂质;然后,再使用UPLC-QqQ-MS优化得到17种杂质的两个定性离子对,并采用多反应监测模式同时对17种杂质进行半定量分析;随后,通过欧几里得距离计算方法对6起制毒案件缴获的112份氯胺酮样品进行聚类分析,验证该方法的可靠性;最后,对700份缴获的氯胺酮进行关联性判别,筛选出14组关联性极强的案件,从而推断出缴获氯胺酮的来源(制毒加工厂)和贩运路线。通过聚类分析及关联性判别得出的结果,可为公安执法部门提供具有科学价值的情报,诸如追溯氯胺酮来源(制毒加工厂)、氯胺酮的贩运路线及串并案分析。

A new method combining ultra-high performance liquid chromatography(UPLC),two types of tandem mass spectrometry,namely quadrupole-time of flight mass(Q-TOF MS)and triple quadrupole-mass(QqQ-MS),and a data analysis technique was developed to profiling the impurities in ketamine.Firstly,the retention times and molecular formulas of 17 characteristic impurities were determined by UPLC-Q-TOF MS.Secondly,two pairs of precursor/products were optimized for each impurity with QqQ-MS,and the responses of 17 impurities were acquired simultaneously in the multiple reaction monitoring(MRM)mode for semi-quantitative analysis.Then,a data set of 112 ketamine samples seized in 6 manufacture cases was obtained and modeled with hierarchical clustering analysis(HCA),which verified the reliability of this methodology.Finally,correlation analysis has been done among 700 ketamine samples,and 14 groups of highly correlated cases has been sorted out,which helped to trace the origin of ketamines(clandestine laboratory)and their traffic network.This methodology can be employed to provide valuable intelligence for law enforcement agencies to trace the clandestine laboratory of ketmine,to establish trafficking routes/distribution patterns and conspiracy links.