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高效液相色谱-串联三重四级杆质谱法测定土壤中苦味酸和联苯胺
Determination of Picric Acid and Benzidine in Soil by High Performance Liquid Chromatography-Tandem Triple Quadruple Bar Mass Spectrometry
投稿时间:2019-04-11  修订日期:2019-07-02
DOI:10.19316/j.issn.1002-6002.2020.04.18
中文关键词:  高效液相色谱-串联三重四级杆质谱  苦味酸  联苯胺  碱性木素  生物质炭
英文关键词:high performance liquid chromatography-tandem triple quadruple bar mass spectrometry  picric acid  benzidine  kraft lignin  bio-charcoal
基金项目:
作者单位
杨静 上海市奉贤区环境监测站,上海200499 
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中文摘要:
      为测定被污染土壤中的低浓度苦味酸和联苯胺,研究建立了一种基于高效液相色谱-串联三重四级杆质谱检测技术的分析方法,实现了超声波乙酸乙酯溶剂萃取后直接进样的高效定性和定量检测。研究表明,在0.5~100.0 μg/L质量浓度范围内,目标化合物的线性关系良好(r>0.999 9),苦味酸、联苯胺的检出限分别为0.16、0.30 μg/kg,精密度相对标准偏差为1.5%~5.8%,加标回收率范围为70.1%~111.0%。该方法灵敏度高、前处理步骤简便,适用于低含量苦味酸和联苯胺的土壤测定。实验表明,以碱性木素为原料,采用热解法在氮气氛围下600℃煅烧得到的生物质炭,对土壤中联苯胺的去除率高达98.2%,对苦味酸的去除率超过50%,可有效实现污染土壤的修复。
英文摘要:
      A method was developed for the determination of low concentration picric acid and benzidine in contaminated soil by high performance liquid chromatography-tandem triple quadruple bar mass spectrometry.The high-efficiency qualitative and quantitative soil detection were realized by direct ultrasonic ethyl acetate extraction.The results showed that good linear relationships with correlation coefficient >0.999 9 were obtained in the mass concentration range of 0.5-100.0 μg/L.The limits of detection (LODs) for picric acid and benzidine were 0.16 and 0.30 μg/kg,respectively.The relative standard deviations (RSD) was 1.5%-5.8% and recovery ranged 70.1%-111%.The presented method was high sensitivity with simple pretreatment steps,and successfully applied to quantify the picric acid and benzidine in soil.The removal rate of bio-charcoal which was prepared from kraft lignin by pyrolysis at 600℃ in nitrogen atmosphere for benzidine was up to 98.2%,and picric acid was over 50%,which realized an effective rehabilitation for contaminated soil.
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