快速溶剂萃取-固相萃取净化/气相色谱-质谱法测定土壤和沉积物样品中65种半挥发性有机物

Determination of 65 SVOCs in Soil and Sediment by Gas Chromatography-Mass Spectrometry with Accelerated Solvent Extraction and Solid Phase Extraction

采用快速溶剂萃取法,结合固相萃取小柱净化,建立了土壤和沉积物样品中65种半挥发性有机物的气相色谱-质谱检测方法。经过前处理条件优化,样品用二氯甲烷∶丙酮(1∶1)为萃取剂进行快速溶剂萃取,稀释后分取10.0 mL萃取液经硅酸镁小柱一次性净化,氮吹仪浓缩。目标物经HP-5MS UI色谱柱分离,选择离子(SIM)模式扫描,选用内标法定量测定。结果表明,方法检出限范围为0.02~0.08 mg/kg,土壤样品加标回收率范围为46.5%~134%,相对标准偏差在0.37%~13.6%范围内。沉积物样品加标回收率范围为48.2%~131%,相对标准偏差在2.8%~18.3%范围内。该方法前处理时间短、检出限低、准确可靠、检测效率高,一次净化即可分析测定所有目标物,可满足土壤和沉积物中65种半挥发性有机物的高通量检测要求。

A gas chromatography-mass spectrometry method for determination of 65 semi-volatile organic compounds(SVOCs)in soil and sediment by accelerated solvent extraction(ASE)with solid phase extraction(SPE)column clean up.The pretreatment was carried out,the samples were extracted with dichloromethane-acetone(1∶1,by volume).After dilution,10.0 mL of the extract was separated and purified by magnesium silicate solid phase extraction column,concentrated by nitrogen blower.The analytes were separated by HP-5MS UI capillary column and scanned with selected ion monitoring(SIM)mode and quantified by internal standard method.The results showed that the detection limits of the method were 0.02~0.08 mg/kg,the average recoveries for soil ranged from 46.5%to 134%,with the relative standard deviations(RSDs)of 0.37%~13.6%,while the average recoveries of sediment were 48.2%~131%,with RSDs of 2.8%~18.3%.The method has the advantages of short pretreatment time,low detection limits,accurate,reliable and high detection efficiency while all the analytes can be purified at one time,which could meet the requirements of high throughput detection of 65 SVOCs in soil and sediment.