气相色谱-质谱法测定土壤中多环芳烃及有机氯农药

Determination of Polycyclic Aromatic Hydrocarbons and Organochlorine Pesticides in soil by Gas Chromatography-triple Quadrupoli Mass Spectrometry

根据国内外研究现状及国家标准《GB15618-1995土壤环境质量标准》《HJ805-2016土壤和沉积物多环芳烃的测定气相色谱-质谱法》,选择土壤中8种有机氯及16种多环芳烃作为研究对象,对土壤样品中有机物的两种前处理技术、溶剂选择、两种不同目数基质分散剂进行分析对比。最终确定:以快速溶剂萃取为基础,60目硅藻土作为基质分散剂,用丙酮∶正己烷(1∶1)作为萃取液,体积比为99%时萃取4次后,经弗罗里硅土柱净化,气相色谱-三重四级杆质谱的检测方法。该方法回收率为49.92%~128.28%,检出限为0.00109~0.00651 mg/kg,满足实际分析要求。

According to national standards of soil environmental quality standard(GB 15618-1995)and the determination of polycyclic aromatic hydrocarbons in soil and sediments by gas chromatography-mass spectrometry(HJ 805-2016),8 kinds of organochlorine pesticides(OPCs)and 16 of polycyclic aromatic hydrocarbons(PAHs)in soil were selected as the research objects.Two pretreatment techniques,solvent selection and two different matrix dispersants for organic matter detection in soil samples were analyzed and compared.The gas chromatograph-three weight four lever mass spectrometry detection method was as follows based on fast solvent extraction,60 mesh diatomite was used as matrix dispersant,and the rate of acetone and n-hexane(1∶1)was used as extractive solution.After 4 times of extraction when the volume ratio of 99%,it was purified by floret silica column.The recovery rate was 49.92%~128.28%,and the detection limit was 0.00109~0.00651mg/kg,which met the requirements of practical analysis.This method has the characteristics of simple and rapid,and shortens the pretreatment and analysis time.It has reference for the detection of polycyclic aromatic hydrocarbons and organochlorine pesticides in soil.