色谱-质谱联用法测定污水中毒品含量的方法比较

Method comparison for determination of illicit drugs in wastewater by liquid chromatography-spectrometry

污水分析法因其客观、简便等优点,已被越来越多的地方政府用于区域毒情评估。此文建立了高效液相色谱-串联质谱法测定污水中13种毒品及其代谢物和人口标记物,并对离线方法和在线方法进行了比较。离线和在线方法的线性相关系数(R2)均≥0.9970,六次平行测定浓度的相对标准偏差(RSD)分别在0.2~2.5%和0.7~6.7%之间,低、中、高水平的加标回收率分别在88.3~109.8%和98.7~117.6%之间。离线方法对分析仪器的配置和灵敏度要求更低,在样品基质过于复杂、干扰峰难以分辨时更有优势,在线方法的前处理更简单,时间和人力成本更低。将以上方法应用于171个污水处理厂样品中毒品的检测,两种方法的检测结果无显著差别,均能满足污水样品中毒品检测的要求。同时,为了解决某些基质复杂的污水样品检测时存在干扰的问题,还介绍了一种针对特殊污水样品的毒品准确定量的色谱分析思路和策略,以提高方法的通用性、准确性和分析效率,为毒品滥用情况评估提供可靠、高效的分析手段。

There is a new technology to monitor the consumption of illicit drugs,which use the content of drugs and their metabolites as well as population markers in wastewater.It is more objective,and is used by more and more local governments.In this paper,a high-performance liquid chromatography-tandem mass spectrometry method was established for the determination of 13 illicit drugs,their metabolites and population markers in wastewater,and the offline and online methods were compared.The linear correlation coefficients of both offline and online methods were≥0.9970,and the relative standard deviations(RSDs)of precision test were between 0.2~2.5%and 0.7~6.7%,respectively.The spiked recoveries of low,medium,and high levels were between 88.3~109.8%and 98.7~117.6%,respectively.The offline method has lower requirements on the configuration and sensitivity of the analytical instrument.Moreover,it also possesses more advantages when the sample matrix is too complex and the interference peaks are difficult to resolve.The online method needs simpler pretreatment,less time consuming and lower labor costs.The above methods were applied to the determination of illicit drugs in 171 sewage treatment plant samples.The results of the two methods have no significant difference,which both met the requirements for the detection of illicit drugs in wastewater.Furthermore,in order to resolve the interference in the detection of special wastewater samples,a chromatographic analysis strategy for the accurate quantification of illicit drugs is also introduced.It is expected to improve analysis efficiency,reduce analysis cost,improve accuracy and universality of the method,and then provides a reliable and efficient analytical tool for assessing illicit drug abuse.