超声波提取-气相色谱质谱联用法测定土壤中23种邻苯二甲酸酯

建立了超声波提取-气相色谱-质谱联用技术分析土壤中23种邻苯二甲酸酯(Phthalic acid esters,PAEs)的新方法.以V(二氯甲烷)∶V(丙酮)=1∶1混合溶液作提取剂分两次超声提取,每次提取10 min,使用硅胶(SI)及N-丙基乙二胺(PSA)两种固相萃取小柱串联净化,使用HP-5MS色谱柱,在26 min内23种PAEs分离良好,且23种PAEs具有良好的线性关系,相关系数不小于0.990,平均加标回收率为81.1%~109.2%,相对标准偏差为3.6%~11.9%,检出限为0.90

Determination of 23 PAEs in soil by GC/MS and ultrasonic wave extraction

A new method was developed for the determination of twenty-three phthalic acid esters （PAEs） in soil by ultrasonic wave extraction coupled with gas chromatography-mass spectrometry. The extraction conditions were optimized. A good extraction efficiency was obtained by using mixed solvent of V （dicbloromethane） ：V （acetone） = 1：1 as extraction solvent, ultrasonic wave extraction twice, 10 minutes each extraction. The extract was cleaned up by silica gel connected with PSA solid phase extraction columns. The chromatographic conditions were optimized by HP-5MS column, twenty-three kinds of PAEs in well separated within twenty-six minutes. Qualitative detection and confirmation were acquired by extraction of characteristic ions, the interferences due to the complex matrixes in soil were effectively eliminated, to avoid the possibility of false positive results. The calibration curves for 23 PAEs all had good linear relationships with correlation coefficients over 0. 990. The average spiked recoveries ranged from 81. 1% to 109. 2% with relative standard deviations of 3.6% - 11.9%. The limits of detection were in the range of 0.90 - 40 ng/g. The method was applied in the determination for PAEs in soil with satisfactory results.