固相萃取/液质联用法检测污水中14种毒品及代谢物

Solid Phase Extraction/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of 14 Drugs and Their Metabolites in Wastewater

建立了采用固相萃取/液质联用法检测污水中14种常见毒品及其代谢物的分析方法。水样经MCX固相萃取柱富集后,用超纯水净化,再分别使用甲醇与5%氨水甲醇溶液洗脱,氮吹定容后,采用液相色谱-串联质谱进行检测。结果表明,吗啡等14种常见毒品及其代谢物在1.0~500 ng/L、人口标记物可替宁在10~5 000 ng/L范围内线性良好,R^(2)>0.999,方法对毒品及其代谢物的检出限(S/N=3)为0.2~0.5 ng/L,污水加标回收率范围为70.00%~115.57%。应用该方法对湖南省8家污水处理厂的进水口污水进行了检测,验证了该方法的可靠性,为进一步研究区域毒品滥用情况评估方法提供了参考依据。

This paper established a method of solid phase extraction/ultra performance liquid chromatography-tandem mass spectrometry for determination of 14 common drugs and their metabolites in wastewater. Wastewater samples were enriched by MCX solid phase extraction column, purified with ultrapure water, and eluted with methanol and 5% ammonia methanol solution respectively. After nitrogen blowing, ultra performance liquid chromatography-tandem mass spectrometry was used for detection. The linearity of 14 common drugs and their metabolites was good when their concentrations were in the range of 1.0-500 ng/L and population marker cotinine was in the range of 10-5 000 ng/L. The correlation coefficient R^(2) was greater than 0.999, the detection limit(S/N of 3) of drugs and their metabolites was 0.2-0.5 ng/L, and the spike recovery rate of wastewater ranged from 70.00% to 115.57%. The method was applied to detect the inlet wastewater of 8 sewage treatment plants in Hunan Province, and the reliability of the method was verified, which provided a reference for further establishment of regional drug abuse assessment methods.