摘要
目的 建立一种应用固相萃取-超高效液相色谱串联质谱法(SPE-UPLC-MS/MS)对城市污水中氟胺酮及2种位置异构体(3F-DCK、4F-DCK)进行定性、定量分析的方法。方法 城市污水以12 000 r/min离心5 min,经过1.2μm玻璃纤维滤膜过滤,加入氯胺酮-D4内标,使用CNW Poly-Sery MCX固相萃取柱净化富集,并复溶于100μL甲醇中。采用岛津GL Sciences Intersil HILIC(3.0mm×150mm,3μm)色谱柱对氟胺酮及2种位置异构体进行色谱分离,以体积比为98∶2的乙腈-10 mmol/L乙酸铵为流动相进行等度洗脱,采用电喷雾离子源正离子模式和多反应监测模式检测。结果 氟胺酮及2种位置异构体在1.0~80.0 ng/L内线性关系良好(相关系数大于等于0.999);氟胺酮、3F-DCK、4F-DCK的检出限分别为0.2、0.3、0.4 ng/L;日内精密度和日间精密度均小于8.1%,方法回收率为69.5%~108%。结论 建立了氟胺酮及2种位置异构体的SPE-UPLC-MS/MS分析方法,可同时对城市污水样品中的氟胺酮及2种位置异构体进行准确的定性、定量分析,并应用于实际样品的检测。
Objective To establish a method for the qualitative and quantitative analysis of 2-fluoro deschloroketamine(2-FDCK), and its two positional isomers, 3F-DCK and 4F-DCK in urban sewage samples by solid phase extraction-ultra high performance liquid chromatography tandem mass spectrometry(SPE-UPLC-MS/MS). Methods The urban sewage sample was first centrifuged at 12 000 r/min for 5 min, filtered through 1.2 μm glass fiber filter, and purified and concentrated by a CNW poly-SERY MCX SPE column, with ketamine-D4as the internal standard. Then it was re-dissolved in 100 μL of methanol.2-FDCK, 3F-DCK and 4F-DCK were separated on a Shimadzu GL Sciences Intersil HILIC column(3.0 mm×150 mm, 3 μm).Acetonitrile-10 mmol/L ammonium acetate was used as the mobile phase for isocratic elution. The electrospray ion source was operated in the positive ion mode. Multiple reaction monitoring(MRM) mode was used for the qualitative and quantitative analysis. Results The analytes had good linear relationship in the range of 1.0-80.0 ng/L(correlation coefficient r≥0.999). The limit of detection for 2F-DCK, 3F-DCK and 4F-DCK were 0.2 ng/L, 0.3 ng/L and 0.4 ng/L, respectively.The intra-day and inter-day precision were less than 8.1 %, and the recovery ranged from 69.5 % to 108 %. Conclusion A SPE-UPLC-MS/MS method was established and validated for the simultaneous determination of 2-FDCK and its two positional isomers, 3F-DCK and 4F-DCK. It can provide accurate analysis of 2-FDCK, 3F-DCK and 4F-DCK at the same time in sewage samples.
作者
王平
刘晓云
郑振成
梁桂巧
赖胜强
WANG Ping;LIU Xiaoyun;ZHENG Zhencheng;LIANG Guiqiao;LAI Shengqiang(Guangdong Accurate and Correct Institution of Forensic Science,Guangzhou Accurate and Correct Test Co.,Ltd,Guangzhou 510663,China)
出处
《中国司法鉴定》
2022年第5期67-72,共6页
Chinese Journal of Forensic Sciences
