加速溶剂萃取(ASE)气相色谱-质谱法测定土壤中的6种硝基苯化合物  

Gas Chromatography-Mass Spectrometry Determination of Six Kinds of Nitrobenzene Compounds in Soil With Accelerated Solvent Extraction

作　　者：陈秀娜[1] 张建民 张明[1] 吴哲[1] 王平平 刘海英[1] CHEN Xiu-na;ZHANG Jian-min;ZHANG Ming;WU Zhe;WANG Ping-ping;LIU Hai-ying(Qinghai Province Geology Ore Testing and Application Center,Qinghai Xining 810008,China;Qinghai Province Product Quality Supervision and Inspection Institute,Qinghai Xining 810008,China)

机构地区：[1]青海省地质矿产测试应用中心,青海西宁810008 [2]青海省产品质量监督检验所,青海西宁810008

出　　处：《当代化工》2018年第10期2228-2231,共4页Contemporary Chemical Industry

摘　　要：提出了加速溶剂萃取-气相色谱-质谱法测定土壤中6种硝基苯类化合物的方法。样品通过ASE萃取后脱水浓缩,经Florisil固相萃取小柱净化测定。在气相色谱分离中用TG-5MS石英毛细管色谱柱为固定相,在质谱分析中采用选择离子监测(SIM)模式,采用内标法定量。该方法的校准曲线的线性良好,样品中各组分曲线相关系数R2均大于0.9950,6种硝基苯类化合物的检出限为0.18～0.80μg·kg^(-1),平均回收率在52.7%～122.4%,相对标准偏差(n=7)在3.14%～6.52%之间,适合测定土壤中的6种硝基苯类化合物。A method for determination of six kinds of nitrobenzene compounds in soil with accelerated solvent extraction-gas chromatography mass spectrometry was established. The samples were dehydrated and concentrated after extraction by ASE,and were purified by Florisil solid phase extraction column. TG-5 MS quartz capillary column was used as fixed phase in gas chromatographic separation. SIM pattern was used in mass spectrometry. The internal standard method was used to quantify. The calibration curve of this method was linear and the correlation coefficient of each component curve of R2 was greater than 0.995 0, and the detection limits of six kinds of nitrobenzene compounds were 0.18～0.80 μg·kg（-1）, the average recovery was 52.7%～122.4%,and the relative standard deviation（n=7） was between 3.14%～ 6.52%. This method is suitable for determination of six kinds of nitrobenzene compounds in soil.

关 键 词：硝基苯 气相色谱-质谱 加速溶剂萃取 

分 类 号：O657.63[理学—分析化学]