基质固相分散萃取-气相质谱联用法测定土壤中19种苯胺类物质

Determination of 19 Aniline Compounds in Soil by Matrix Solid Phase Dispersion-GCMS

采用基质固相分散萃取结合GCMS法,选择弗罗里硅土为分散剂,样品与分散剂比例为1∶4,正己烷∶丙酮(1∶1)为洗脱剂,建立了一种快速、准确测定土壤中19种苯胺类物质的方法。结果表明:19种苯胺类化合物的线性范围为0.1~10mg/L,相关系数(R)在0.9973~0.9999,3个浓度梯度下方法平均回收率87.3%~109%,相对标准偏差(n=6)为0.796%~4.91%,方法检出限为0.017~0.075mg/kg。该方法简便可行,灵敏度、准确度和精密度均可以满足土壤中19种苯胺类物质的检测要求。

A rapid and accurate method was developed for the determination of 19 aniline compounds in soil. MSPD and GCMS were employed for the analysis, florisil was selected as the extraction adsorbent, the mass ratio of sample to dispersant at 1：4, a mixture of 1 ：1 （V ： V ） acetone： hexane as eluting solvent, and 30m L eluent volume . Chromatographic column was HP - 5 M S （30 m ×0 . 25 m m ×0 . 25 μ m ） with column temperature of 40℃ for 2 min, 10℃/min to 260℃ for 10 min, injection temperature was 260℃ , split ratio was 5：1, flow rate was 1 m L / min, El source temperature was 230℃, transmission line temperature was 280℃ , ionization energy was 70 e V . The results showed that the correlation coefficient （R ） was 0.9973 -0.9999 when the concentration was among 0. 1 -10mg/L,the recovery rate was among 87. 3 % -109% for three concentration series, the R S D was 0-796% -4. 91 %,the detection limit of the 19 aniline compounds were 0-017m g / k g ？075m g/kg. The method is appli-cable. Its sensitivity, accuracy and prevision all met the analysis requirement.