毛发中氯胺酮及其代谢物LC-MSMS检验方法研究

Study on the Test Method of Ketamine and Its Metabolites LC-MS/MS in Hair

目的:建立毛发中氯胺酮及其代谢物去甲氯胺酮的液相色谱-串联质谱(LC-MS/MS)检验方法。方法称取毛发样品20 mg,依次用去离子水、丙酮等洗净,晾干,置含陶珠的毛发毒品检测提取试剂管中,用含内标氯胺酮-D_(4)、去甲氯胺酮-D_(4)的甲醇∶水(1∶1,体积比)溶液研磨提取,提取液用0.22μm微孔有机滤膜过滤,用LC-MS/MS检测。结果氯胺酮在0.01~50 ng/mg质量范围内线性关系良好(r^(2)=0.9923),检出限0.005 ng/mg,定量限0.01 ng/mg;去甲氯胺酮在0.01~50 ng/mg质量范围内线性关系良好(r^(2)=0.9973),检出限0.005 ng/mg,定量限0.01 ng/mg。结论所建立的毛发中氯胺酮及其代谢物去甲氯胺酮LC-MS/MS检验方法操作简便、检测灵敏度较高,可用于公安实际氯胺酮吸食案件中氯胺酮及其代谢物去甲氯胺酮的检验。

Objective:To establish a method for the determination of ketamine and its metabolite norketamine in hair by liquid chromatography tandem mass spectrometry(LC-MS/MS).Method:Weigh 20 mg of hair sample,which wash it with deionized water and acetone,dry it in the air,and put it into the hair drug detection and extraction reagent tube containing ceramic beads,the extraction was carried out by grinding with methanol∶water(1∶1)solution containing internal standard ketamine-D_(4) and norketamine-D_(4),0.22μm microporous organic filter membrane filtration,LC-MS/MS detectio.Results Ketamine has a good linear relationship in the mass range of 0.01~50 ng/mg(r^(2)=0.9923),check out 0.005 ng/mg,quantitative limit of 0.01 ng/mg;noreketamine has a good linear relationship in the mass range of 0.01~50 ng/mg(r^(2)=0.9973),check out 0.005 ng/mg,quantitative limit of 0.01 ng/mg.Conclusion The test method of ketamine and its metabolites in hair LC-MS/MS is simple in operation and has high detection sensitivity.It can be used for the test of ketamine and its metabolite nucloamine in actual ketamine smoking cases.