微波萃取-SPE柱净化/气相色谱-质谱法测定固体废物中53种半挥发性有机物  

Determination of 53 Semi-volatile Organic Compounds in Solid Waste by Gas Chromatography-Mass Spectrometry with Microwave Extraction and Solid Phase Extraction Column Purification

作　　者：蒋建军 卢光磊 刘丽 向勇 JIANG Jian-jun;LU Guang-lei;LIU Li;XIANG Yong(Hunan Division of GRG Metrology and Test,Changsha 410000,China)

机构地区：[1]广电计量检测(湖南)有限公司,湖南长沙410000

出　　处：《分析测试学报》2023年第4期464-472,共9页Journal of Instrumental Analysis

基　　金：湘江流域区域产地镉砷污染活化及调控机制课题资助(2022YFD1700102)。

摘　　要：采用微波辅助萃取技术,结合固相萃取(SPE)小柱净化,建立了固体废物中53种半挥发性有机物的气相色谱-质谱检测方法。通过优化前处理条件,选择以丙酮-正己烷(1∶1,体积比)为萃取剂,微波萃取温度为100℃,萃取时间为15 min,萃取液经硅酸镁固相萃取柱净化,DB-5MS(30 m×0.25μm×0.25 mm)色谱柱分离,结合电子轰击电离源(EI)选择离子监测(SIM)模式,采用内标法进行定量检测。实验表明:53种半挥发性有机物在0.2~5.0 mg/L范围内线性良好,相关系数(r)均不小于0.998,对典型固体废物灰渣和生化污泥样品的检出限分别为0.002~0.015 mg/kg和0.004~0.027 mg/kg,定量下限分别为0.008~0.060 mg/kg和0.016~0.108 mg/kg。在0.5、1.0、2.0 mg/kg 3个加标水平下,灰渣样品的平均加标回收率为70.7%~98.5%,相对标准偏差(RSD,n=6)为1.7%~14%;生化污泥样品的平均加标回收率为71.8%~105%,RSD(n=6)为1.2%~15%。该方法快速准确、环保可靠、试剂用量少、检测效率高,可满足固体废物中53种半挥发性有机物的高通量检测要求。A gas chromatography-mass spectrometry(GC-MS)was established for the determina⁃tion of 53 semi-volatile organic compounds in solid wastes,based on microwave-assisted extraction combined with solid phase extraction(SPE)column cleanup.Extraction was carried out in a micro⁃wave extraction tank using 20 mL acetone-hexane(1∶1,by volume)as the extractant,with an ex⁃traction temperature of 100℃and an extraction time of 15 min,then the extract was concentrated by nitrogen blowing.The analyte was purified by magnesium silicate solid phase extraction column and separated on a DB-5MS(30 m×0.25μm×0.25 mm)capillary column,finally detected with elec⁃tron bombardment ionization source(EI)in selected ion monitoring(SIM)mode and quantified by in⁃ternal standard method.The results showed that there were good linear relationships for 53 semi-vola⁃tile organic compounds in the range of 0.2-5.0 mg/L,with their correlation coefficients(r)not less than 0.998.The limits of detection for typical solid waste ash and biochemical sludge samples were in the range of 0.002-0.015 mg/kg and 0.004-0.027 mg/kg,while the limits of quantitation were in the range of 0.008-0.060 mg/kg and 0.016-0.108 mg/kg,respectively.For two typical solid waste negative sample matrices,the average recoveries at three spiked levels of 0.5,1.0 and 2.0 mg/kg for ash sample ranged from 70.7%to 98.5%,with relative standard deviations(RSDs,n=6)of 1.7%-14%,while the average recoveries for biochemical sludge sample ranged from 71.8%to 105%,with RSDs(n=6)of 1.2%-15%.The method was applied to the analysis of solid waste sam⁃ples from Miluo pesticide plant,in which seven semi-volatile organic compounds,i.e.phorate,fenitrothion,heptachlor,hexachlorobenzene,p,p'-DDE,p,p'-DDT and mirex with different con⁃centrations were detected.This method is rapid,accurate,environmentally friendly and reliable,and low reagent consumption,which could meet the requirements for high throughput detection of 53 semi-volatile organic compounds in solid waste,and significantly

关 键 词：半挥发性有机物 固体废物 微波萃取 固相萃取 气相色谱-质谱联用 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]