酸碱净化-改进的衍生化气相色谱/质谱法测定土壤中11种酚类化合物

Determination of 11 Phenolic Compounds in Soil by Acid-base Purification-modified Derivatization Gas Chromatography/Mass Spectrometry

实现了土壤经有机溶剂快速提取,经酸碱净化,采用改进的五氟苄基溴方法衍生后,建立了气相色谱-质谱法同时测定土壤中11种酚类化合物的新方法。目标化合物通过SIM方式扫描,对保留时间和特征离子定性,通过内标法定量。土壤采用二氯甲烷/正己烷共同提取后,在酸碱净化过程中优化了不同萃取溶剂比例和不同体系下五氟苄基溴衍生效果的影响,以及考查了不同衍生温度和时间的作用。当取样量10 g时,11种酚类化合物方法检出限为1.06~4.21μg/kg,低、中、高基质加标回收率为75.9%~93.9%,相对标准偏差(RSDs)为4.6%~8.2%。

A new method was developed for the simultaneous determination of 11 phenolic compounds in soil by gas chromatography-mass spectrometry(GC-MS)after rapid extraction with solvent,purification with acid and alkali,derivatization with improved pentafluoro-benzyl bromide.The target compounds were scanned by SIM method,the retention time and characteristic ions were characterized,and quantitative by internal standard method.After the extraction of dichloromethane/hexane,the effects of different extraction solvent ratio and different system on the derivatization of pentafluorobenzyl bromide were optimized in the process of acid-base purification,and the effects of different derivatization temperature and time were investigated.When amount of the sample was 10 g,the detection limits of 11 phenolic compounds were 1.06~4.21μg/kg,the recoveries of low,medium and high matrix were 75.9%~93.9%,and the relative standard deviations(RSDs)were 4.6%~8.2%.