加速溶剂萃取-气相色谱/质谱法分析土壤中的酞酸酯

建立了用加速溶剂萃取法（ASE）提取、气相色谱-质谱法分析土壤中6种酞酸酯的方法。分析了空白值的来源及其控制方法。较佳实验条件为：用二氯甲烷和丙酮（1：1,v/v）的混合溶剂为提取剂,萃取温度120℃,压力1500psi,静态提取10min,循环提取2次。选择离子模式下监测,线性范围：20μg/L-1000μg/L,平均加标回收率在88%-123%之间,相对标准偏差小于14.2%,检出限5～15ng。标准土壤样品的测试结果与索氏提取、超声波提取法进行了比较,测定误差表明：三种方法测定结果均在可接受范围内,ASE法的测定结果和索氏提取法相近,其统计值的误差较超声波提取法的测定结果小。ASE方法耗时少,有机溶剂用量小,干扰少,自动化程度高,重现性好,回收率高。

Determination of Phthalate Esters in Soil using Accelerated Solvent Extraction and Gas Chromatography-Mass Spectrometry

A method is established for the simultaneous determination of 6 phthalate esters,namely,dimethyl-phthalate（DMP）,diethyl-phthalate（DEP）,dibutyl-phthalate（DBP）,benzyl-n-butyl phthalate（BBP）,di-（2-ethylhexyl） phthalate（DEHP） and di-octyl phthalate（DOP） in soil by accelerated solvent extraction（ASE） coupled with gas chromatography-mass spectrometry（GC-MS）.The factors related to blank value is discussed and the ways to reduce blank interference are established.Extraction conditions of ASE were optimized as follow： methylene dichloride： acetone（v：v,1：1）was used as extracting solvent;extraction temperature： 120°C;extraction pressure：1500 psi;static extraction time：10min and cycle times：2.Good linearities were observed in the range from 20 to 1000μg/L.The average recoveries ranged from 88% to 123% and the relative standard deviations were less than 14.2%.Satisfying result of testing a soil reference material by ASE was obtained compared with Ultrasonic assisted extraction and Soxhlet extraction.The detection limits were less than 15 ng.The method is simple,sensitive and accurate,and can be easily implemented for monitoring 6 PAEss in soil.