PSE-UPLC-MS/MS法测定污泥中9种药物与个人护理品

Determination of Nine Pharmaceutical and Personal Care Products in Sludge by PSE Coupled to UPLC-MS/MS

利用加压溶剂萃取法(PSE)提取、固相萃取法净化并结合超高效液相色谱-串联四极杆质谱仪(UPLC-MSMS)检测,建立了污水处理厂污泥中7个药剂类别的9种药物与个人护理品(舒必利、咖啡因、美托洛尔、氯霉素、萘啶酸、卡马西平、驱蚊胺、氯贝酸、苯扎贝特)的分析检测方法.在萃取方法中,对加压溶剂萃取的污泥质量和溶剂进行了优化;在净化方法中,对固相萃取柱种类、固相萃取柱容量、洗脱溶剂和洗脱量进行了优选.结果表明,方法检出限(以干质量计,下同)在2.7～65.0 pg/g范围内,加标回收率在67.0%～130%之间,相对标准偏差均小于25%(即标准偏差小于25μg/L).应用所建立的分析方法,对北京某污水处理厂的脱水污泥进行了测定,9种目标物质含量为nd(未检出)～50.5 ng/g,其中,舒必利、咖啡因、卡马西平、驱蚊胺和氯贝酸在2010年春、夏季2次采样均有检出.

A method for the determination of nine pharmaceuticals and personal care products（PPCPs） from seven therapeutic classes（sulpiride,caffeine,metoprolol,chloramphenicol,nalidixic acid,carbamazepine,N,N-diethyl-m-toluamide,clofibric acid and bezafibrate） in sewage sludge was established.Pressurized solvent extraction（PSE） and solid phase extraction（SPE） were employed as the extraction and cleanup methods,respectively,while ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS MS） was used for detection.For the extraction method,the amount of sludge and the extraction solvent were optimized,while for the cleanup method,type and capacity of SPE cartridge and type and volume of elution solvent were optimized.The results showed that the method detection limits（MDLs） ranged from 2.7 to 65.0 pg g（DW）,the spiked recovery ranged from 67.0% to 130%,and the relative standard deviations（RSD） were all below 25%（i.e.the standard deviations were below 25 μg L.With the established method,the concentrations of the nine PPCPs were determined in dewatered sludge samples collected from a wastewater treatment plant in Beijing.The concentrations ranged from no detection to 50.5 ng g（DW）.Sulpiride,caffeine,carbamazepine,N,N-diethyl-m-toluamide,and clofibric acid were detected in the samples collected both in the spring and summer of 2010.