加压流体萃取/液液萃取-气相色谱质谱法测定固体废物中的11种硝基苯类  

Determination of nitrobenzene compounds in solid waste by pressurized fluid extraction/liquid-liquid extraction-gas chromatography mass spectrometry

作　　者：邓维 龚娴 徐义邦 DENG Wei;GONG Xian;XU Yi-bang(Jiangxi Nanchang Ecological Environment Monitoring Center,Nanchang 330038,China)

机构地区：[1]江西省南昌生态环境监测中心,江西南昌330008

出　　处：《化学研究与应用》2023年第8期1966-1973,共8页Chemical Research and Application

摘　　要：建立了加压流体萃取/液液萃取-气相色谱质谱法测定固体废物中11种硝基苯类的方法。以二氯甲烷-正己烷(1∶1)为萃取溶剂,在100℃和100bar条件加压萃取固体废物试样;以二氯甲烷为溶剂,液液萃取固体废物浸出液,萃取液均经硅酸镁固相萃取柱净化,DB-5MS毛细色谱柱分离,气相色谱质谱法检测。优化了前处理和分析过程的重要条件。方法检出限为0.05~0.10mg·kg^(-1)(灰渣)、0.3~0.9mg·kg^(-1)(生化污泥)、0.2~0.3mg·L^(-1)(浸出液),低中高三个浓度的加标回收率范围为52.0%~88.0%(灰渣)、54.0%~84.0%(生化污泥)、55.0%~85.0%(浸出液),精密度为3.8%~8.6%(灰渣)、3.7%~9.1%(生化污泥)、3.5%~9.1%(浸出液),单个目标物的相对标准偏差(RSD)均<10%(n=6)。实验结果表明,该方法简便、可靠,适用于固体废物中11种硝基苯类的测定。A method for the determination of 11 nitrobenzene compounds in solid waste by pressurized fluid extraction·L^(-1)iquid-liquid extraction-gas chromatography mass spectrometry was established.With dichloromethane n-hexane(1∶1)as the extraction solvent,solid waste samples were extracted by pressurized fluid at 100℃and 100 bar;With dichloromethane as the solvent,liquid-liquid extraction of solid waste lixivium was carried out.The extraction solution was purified by magnesium silicate solid phase extraction column,separated by DB-5MS capillary chromatographic column,and detected by gas chromatography-mass spectrometry.The important conditions of pretreatment and analysis process were optimized.The detection limit of the method was 0.05~0.10mg·kg^(-1)(ash),0.3~0.9mg·kg^(-1)(biochemical sludge),0.2~0.3mg·L^(-1)(leaching solution).The range of recovery rates for spiking at low,medium and high concentrations was 52.0%~88.0%(ash),54.0%~84.0%(biochemical sludge),55.0%~85.0%(leaching solution).The precision was 3.8%~8.6%(ash),3.7%~9.1%(biochemical sludge),3.5%~9.1%(leaching solution).The relative standard deviation(RSD)of a single target was less than 10%(n=6).The experimental results showed that the method was simple and reliable,and was suitable for the determination of 11 nitrobenzene compounds in solid waste.

关 键 词：固体废物 加压流体萃取 气相色谱质谱法 硝基苯类 

分 类 号：O657.7[理学—分析化学]