加速溶剂萃取-气相色谱-质谱法检测土壤中染料母体偶氮苯和咔唑

Analysis of Pro-dyes Azobenzene and Carbazole by Accelerated Solvent Extraction and Gas Chromatography-mass Spectrometry

建立了土壤中染料母体偶氮苯和咔唑加速溶剂萃取-在线净化检测方法。土壤经石英砂分散后,装入底部有氟罗里硅土粉和石墨炭黑粉的萃取池中,以丙酮-正己烷(V/V,1∶1)为溶剂用加速溶剂萃取仪萃取并同时完成净化,用DB-5MS柱分离,以气相色谱-质谱定性定量检测。考察了萃取溶剂、萃取温度、分散剂、土壤TOC及净化剂等因素的影响,对空白土壤样品进行3种浓度水平的加标试验,其平均回收率为72.0%~113.7%,相对标准偏差在7.6%~15.8%。此方法用于土壤样品的检测,部分样品中有偶氮苯和咔唑检出。

A method that accelerated solvent extraction and in situ purification of pro-dyes,namely azobenzene and carbazole,was carried out in this research.A soil sample,mixed with some silica sand,was placed in the extract cell with fluorine silica powder and graphitized carbon powder;two objectives were extracted by acetone-hexane（V∶V,1∶1）,and in situ purified in the accelerated solvent extractor.Then they were analyzed by gas chromatography-mass spectrometry using a DB-5 MS column.We studied the influence of extracting solvent,temperature,dispersing agent,TOC content.Difference of in situ and off situ purification as well as superiority of composite purification was also discussed in this study.Spiked recoveries of three concentrations ranged from 72.0%～113.7% with relative standard deviation 7.6%～15.8%.Real sample analysis was constructed by this method,and some azobenzene and carbazole were detected.