改良QuEChERS-气相色谱-串联质谱法同时测定土壤中17种邻苯二甲酸酯

Simultaneous Determination of 17 Phthalic Acid Esters in Soil by Gas Chromatography-Tandem Mass Spectrometry with Improved QuEChERS

建立了改良的QuEChERS法,结合气相色谱-串联质谱(GC-MS/MS)检测土壤中17种邻苯二甲酸酯的分析方法。样品用乙腈水溶液提取,NaCl盐析分层,上清液采用磁性氧化石墨烯(Fe_(3)O_(4)-GO)、N-丙基乙二胺(PSA)和无水MgSO_(4)吸附剂分散固相萃取净化,质谱以多反应监测(MRM)模式测定,外标法定量。结果表明,17种邻苯二甲酸酯在一定浓度范围内,线性关系良好,相关系数均在0.9980以上,方法检出限为0.3~3.0μg/kg,定量限为1.0~10.0μg/kg。对土壤样品进行加标回收率试验,17种邻苯二甲酸酯的平均回收率范围为71.3%~92.4%,相对标准偏差小于10.0%(n=6)。本研究所建立的方法具有操作简单、灵敏度高、重现性好等特点,能够快速、准确、可靠地测定土壤中17种邻苯二甲酸酯。

A method was developed for the simultaneous determination of 17 kinds of phthalic acid esters(PAEs)in soil using gas chromatography-tandem mass spectrometry coupled with improved QuEChERS.Samples were extracted by acetonitrile-water and were purified by Fe_(3)O_(4)-GO,PSA and anhydrous magnesium sulfateadsorbent and quantified by external standard method in multiple reactions monitoring mode(MRM).Under the optimized conditions,the target concentrations and peak areas were linearly correlated in the range of concentrations,and the correlation coefficients were greater than 0.9980.The limits of detection and limit of quantification ranged from 0.3 to 3.0μg/kg and 1.0 to 10.0μg/kg.Recovery studies were carried out on three spiking levels and the mean recoveries were 71.3%to 92.4%,with relative standard deviations less than 10.0%(n=6).The proposed method is suitable for quickly,accurately and reliably analyzing 17 PAEs in soil.