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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

     

摘要

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.%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.

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