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加压流体萃取-气相色谱法测定土壤中酞酸酯类化合物 预览

Determination of Phthalate Esters in Soil by Pressurized Fluid Extraction with Gas Chromatography Method
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摘要 建立了土壤中15种酞酸酯的加压流体萃取-弗罗里硅土柱净化-气相色谱测定方法。就萃取条件探讨了溶剂、温度、时间和循环次数对萃取效率的影响,就净化条件探讨了净化柱和洗脱溶剂对萃取效率的影响。根据研究结果,确定萃取条件以二氯甲烷为萃取溶剂,在萃取温度120℃、压强1 500 psi时,预热5 min,静态提取5 min,循环萃取2次,用体积为60%萃取池体积的萃取溶剂冲洗萃取池,之后用氮气吹扫萃取池90 s;净化条件为萃取溶液过弗罗里硅土固相萃取柱净化后,以正己烷∶丙酮(体积比为5∶1)洗脱。15种酞酸酯类化合物加标回收率为67.1%~124%,方法检出限为0.017~0.048 mg/kg。 A method was developed for the determination of 15 kinds of phthalate esters( APEs) in soil by pressurized fluid extraction,Florisil purification and gas chromatography in this study. The effects of extraction solvent,temperature,duration,repeating times,purification column and elution solvent on extraction efficiency were investigated in detail. The results showed that the optimized extraction procedures are circulating extraction of the soil twice with dichloromethane for 5 minutes at each time under the temperature of 120 ℃ degrees and the pressure of 1 500 psi after preheating for 5 minutes,purifying the solvent extract with Florisil column and eluting with Hexane ∶ Acetone( 5 ∶ 1). The average recoveries for 15 kinds of APEs are 67. 1%-124%,and the detection limits are 0. 017-0. 048 mg/kg.
作者 南淑清 张丹 梁晶 熊飙 赵颖 孔海燕 NAN Shuqing, ZHANG Dan, LIANG Jing, XIONG Biao, ZHAO Ying, KONG Haiyan (Henan Environmental Monitoring Center, Zhengzhou 450004, China)
出处 《中国环境监测》 CSCD 北大核心 2017年第3期154-159,共6页 Environmental Monitoring in China
基金 国家高技术研究发展计划(863计划)“化学品暴露和效应评估及监测关键技术”(2013AA06A308)
关键词 土壤 酞酸酯 加压流体萃取 气相色谱 soil phthalate esters pressurized fluid extraction gas chromatography
作者简介 南淑清(1975一),女,河南濮阳人,硕士,高级工程师。
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