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快速溶剂萃取-气相色谱-质谱法测定土壤中15种硝基苯类化合物
引用本文:王桂珍. 快速溶剂萃取-气相色谱-质谱法测定土壤中15种硝基苯类化合物[J]. 中国农学通报, 2018, 34(26): 100-104. DOI: 10.11924/j.issn.1000-6850.casb17070112
作者姓名:王桂珍
作者单位:南水北调中线渠首环境监测应急中心
摘    要:通过气相色谱-质谱法(GC-MS),建立土壤中15 种硝基苯类化合物的快速测定方法,以期为土壤和固体物中硝基苯类化合物残留量的测定提供参考。样品中的15 种硝基苯类化合物经正己烷和丙酮(1:1, V:V)溶剂萃取,硅酸镁小柱净化,10 mL正己烷:丙酮混合溶液(1:1, V:V)洗脱并干燥浓缩后,用GCMS测定,内标法定量。结果表明:此方法线性关系良好,相关系数均大于0.995,15 种硝基苯类化合物的回收率在71.6%~119%之间,相对标准偏差在0.2%~1.1%之间,检出限在0.05~1.31 μg/kg 之间。该方法简便、准确度好、灵敏度高,节约人力财力,满足土壤中硝基苯类化合物的测定要求。

关 键 词:快速溶剂萃取  气相色谱—质谱法  硝基苯类化合物
收稿时间:2017-07-22
修稿时间:2018-08-17

Determination of Nitrobenzene Compounds in Soil by ASE-GC-MS
Abstract:A method was developed for the determination of nitrobenzenes?compound in soil by GC-MS with accelerated solvent extraction. Method of drug samples for nitrobenzenes?compound by acetone and n-hexane(1:1) extraction,solid-phase extraction separation,drying and concentrating,analysis by GC-MS with ASE,internal standard method for the quantitative analysis.The results were present as follows.The method was suitable for the determination of nitrobenzenes?compound using the acetone and n-hexane(1:1) as elution solvent in soil.It had good separation effect and the calibration curves showed good linear relationship. The correlation coefficients >0.995. Samples extracted showed the highest recovery. The recoveries of nitrobenzenes?compound were in range of 71.6%~119% and the relative standard deviations were 0.2%~1.1%. The detection limits were 0.05~1.31μg/kg.The method had merits of simplicity,accuracy,sensitivity and it can meet the test requirements of nitrobenzenes?compound in soil.
Keywords:accelerated solvent extraction   GC-MS  nitrobenzenesScompound
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