液相色谱-串联质谱法同时测定污水中10种精神活性物质

建立了采用液相色谱-串联质谱法(LC-MS/MS)同时测定污水中10种精神活性物质的分析方法。污水样品经甲酸与甲酸铵调节pH后,加入氘代内标混匀,离心并过滤膜后可直接上样分析。研究表明,在1~250 ng/L的线性范围内,10种精神活性物质的线性相关系数均大于0.992,定量限均低于0.5 ng/L。在3个加标水平下,10种精神活性物质的加标回收率为87.2%~114%,相对标准偏差为0.53%~3.60%(n=3)。将该方法应用于某区域10份生活污水样品的检测,在3份水样中检出吗啡、甲基苯丙胺、氯胺酮等精神活性物质,对应的质量浓度范围分别为3.41~9.55、0.90~1.63、1.06~1.78 ng/L。与经固相萃取前处理后的分析方法相比,该方法可在10 min内完成分离和检测的全过程,具有简单、快速、节约的优点,可用于污水样品中10种痕量水平精神活性物质的定量分析。

Simultaneous Determination of 10 Psychoactive Substances in Wastewater by Liquid Chromatography-Tandem Mass Spectrometry

An analytical method was established for simultaneous determination of 10 psychoactive substances in wastewater based on liquid chromatography-tandem mass spectrometry (LC-MS/MS).The pH levels of the collected wastewater samples were adjusted by adding formic acid and ammonium formate,and then the solutions were mixed with deuterated isotope internal standards.The samples could be analyzed by LC-MS/MS directly just after centrifuged and filtered without sample enrichment.The results showed that in the linear range of 1-250 ng/L,the linear correlation coefficients of 10 psychoactive substances were all greater than 0.992,and the limits of quantification were all lower than 0.5 ng/L.At the three spiked levels,the recoveries of 10 psychoactive substances ranged from 87.2% to 114%,while the relative standard deviations (RSD) were between 0.53% and 3.60% (n=3).The method was successfully applied to the determination of 10 wastewater samples in some districts.Morphine,methamphetamine and ketamine were detected in the 3 water samples,with contents in the ranges of 3.41-9.55 ng/L,0.9-1.63 ng/L,1.06-1.78 ng/L,respectively.Compared with the SPE method,this method can complete the whole process of separation and detection within 10 min,which is simpler,rapid and economical without pretreatment,and can be used for the determination of 10 trace levels of psychoactive substances in wastewater.