加压流体萃取-气质联用-内标法测定土壤中24种苯胺类和联苯胺类化合物  

Determination of 24aniline and benzidine compounds in soil by pressurized fluid extraction-gas chromatography-mass spectrometry-internal standard method

作　　者：杨明[1] 付海美 邵鹏[1] YANG Ming;FU Haimei;SHAO Peng(Beijing Center for Physical and Chemical Analysis,Beijing 100089,China)

机构地区：[1]北京市理化分析测试中心,北京100089

出　　处：《分析试验室》2022年第8期940-946,共7页Chinese Journal of Analysis Laboratory

基　　金：北京市科学技术研究院改革与发展项目(2021ZL0116)资助。

摘　　要：建立了加压流体萃取-气质联用-内标法同时测定土壤中24种苯胺类和联苯胺类化合物的分析方法。样品经过加压流体萃取,利用固相萃取柱净化,通过配备DB-5MS毛细管柱(30 m×0.32 mm×0.25μm)的气相色谱-质谱仪分离,离子监测(SIM)模式的条件下,采用内标法定量。24种苯胺类和联苯胺类化合物在0.5~10μg/mL范围内线性良好,相关系数均大于0.995;检出限为0.6~7.6μg/kg,定量限为2.4~30.4μg/kg。选取土壤样品,分别在3个加标水平下验证方法的准确度和精密度,24种苯胺类和联苯胺类化合物的平均回收率为51.6%~119.5%,相对标准偏差为0.3%~4.9%。该方法适用于土壤中苯胺类和联苯胺类化合物的检测。A method for the simultaneous determination of 24 aniline and benzidine compounds in soil was established by pressurized fluid extraction-gas chromatography-mass spectrometry-internal standard method.The sample was extracted with accelerated solvent extraction,and purified with solid phase extraction columns.Then,the aniline and benzidine compounds were separated using gas chromatography-mass spectrometry equipped with a DB-5MS capillary column(30 m×0.32 mm×0.25μm)at selective ion monitoring(SIM)mode,and quantified with the internal standard method.Results showed that good linearities for 24 aniline and benzidine compounds were in the range of 0.5-10μg/mL with the correlation coefficients greater than 0.995,while the limits of detection and limits of quantiatation were in the ranges of 0.6-7.6μg/kg and 2.4-30.4μg/kg,respectively.The soil was selected to verify the accuracy and precision of the method with 3 standard addition levels.The average spiked recoveries ranged from 51.6%to 119.5%and the relative standard deviations were 0.3%-4.9%.The method is suitable for the determination of aniline and benzidine compounds in soil.

关 键 词：加压流体萃取 苯胺类和联苯胺类化合物 内标法 气质联用 

分 类 号：O657.63[理学—分析化学]