顶空固相微萃取与气质联用快速检测尿液中氯胺酮及去甲基氯胺酮

目的建立利用顶空固相微萃取（HS／SPME）结合气相色谱／质谱联用技术（GC／MS）快速检测吸毒人员尿液中氯胺酮（KT）及其主要代谢物去甲基氯胺酮（NK）的方法。方法样品瓶中加入尿样、6mol／L氢氧化钠溶液、固体氯化钠、SKF525A（内标），85℃下加热搅拌，用100μm聚二甲基硅氧烷（PDMS）萃取头顶空萃取10min，GC／MS（EI-SIM）检测。结果尿液中NK和KT浓度在0．1～2．0μg／ml范围内呈现线性关系，相关系数分别为（r^2）0．9991和0．9945，检测限（D／N=3）分别为0．87ng／ml和2．76ng／ml，定量限（S／N=10）分别为2．90ng／ml和18．52ng／ml。1ml尿液加标600ng，NK回收率在85．5％～110．1％，RSD〈13．2％（n=6）；KT回收率在77．5％～109．6％，RSD〈511．99％（n=6）。结论建立的方法简单、快速、灵敏、准确，适合尿液等生物检材中NK及KT的快速定性定量分析。

Detection of ketamine and norketamine in urine by HS/SPME and GC/MS

Objective To establish a method for detecting the KT and its metabolite in the urine of drugger. Method Sample urine, 6 mol/L sodium hydroxide, solid sodium chloride and SKF525A （internal standard solution） were added into vials, stirred and heated to 85~C. The solution was extracted by HS-SPASE with 100μm polydimethylsiloxane （PDMS）, a non-polar coated fiber for 10 minutes and then analyzed by GC/MS（EI-SIM）. Results The calibration curves for the concentration of NK and KT in the urine showed linearity in the range of 0. 1-2.0μg/ml. The respective correlation coefficients （r^2） were 0. 9991 and 0. 9945. The respective detection limits （S/N= 3） were 0. 87ng/ml and 2. 76ng/ml, the qualification limits （S/N= 10） were 2. 90ng/ml and 18.52ng/ml. 600ng NK was added in the lml urine as standard sample, the recovery of NK was in the range of 85.5%-110. 1%, RSD〈13. 2%（n=6）; the recovery of KT was in the range of 77. 5%-109.6%,RSD〈11. 99%（n=6）. Conclusion The method was simple, quick, delicacy , accuracy and suitable for qualititative and quantitative analysis of NK and KT in the biological samples, such as urine etc.