加压流体萃取-气相色谱-质谱法同时测定土壤中10种半挥发性有机物  

Simultaneous determination of 10 semi-volatile organic compounds in soil by pressurized fluid extraction-gas chromatography-mass spectrometry

作　　者：郝杰 孙鹏飞 高玉花 毕建玲 李云龙 张同生 HAO jie;SUN Pengfei;GAO Yuhua;BI Jianling;LI Yunlong;ZHANG Tongsheng(Shandong Institute of Geophysical and Geochemical Exploration,Jinan 250013,China)

机构地区：[1]山东省物化探勘查院,济南250013

出　　处：《化学分析计量》2022年第3期9-13,共5页Chemical Analysis And Meterage

基　　金：山东省地矿局科技攻关项目(KY202109)。

摘　　要：建立加压流体萃取(ASE)-气相色谱-质谱(GC-MS)法同时测定土壤中苯胺、硝基苯和多环芳烃等10种半挥发性有机物(SVOCs)的方法。在土壤中加入适量氨水调节pH值为10.0,以二氯甲烷为萃取溶剂,萃取温度为90℃,循环萃取2次,萃取液真空浓缩后,经0.45μm有机滤膜过滤,采用气相色谱-质谱法进行测定。10种半挥发性有机物与内标物色谱峰面积的比值与质量浓度在1~20 mg/L范围内具有良好的线性关系,相关系数均不小于0.998,方法检出限为0.02~0.06 mg/kg。实际土壤样品的加标回收率为74.2%~95.8%,测定结果的相对标准偏差为1.6%~9.9%(n=6)。该方法满足同时测定土壤中10种半挥发性有机物的要求。A method for simultaneous determination of 10 semi-volatile organic compounds(SVOCs) such as aniline,nitrobenzene and polycyclic aromatic hydrocarbons in soil by gas chromatography-mass spectrometry(GC-MS) with pressurized fluid extraction(ASE) was established. Appropriate amount of ammonia water was added to the soil to adjust the pH to 10.0. Dichloromethane was used as the extraction solvent. The extraction temperature was 90 ℃ and the extraction cycle was twice. The extract was concentrated in vacuum and filtered through 0.45 μm organic filter and determined by GC-MS. The ratio of the chromatographic peak area of the 10 semi-volatile organic compounds to the internal standard substance had a good linear relationship with the mass concentration in the range of 1-20 mg/L, the correlation coefficient were not less than 0. 998 and the detection limits of the method were 0.02-0.06 mg/kg. The average recoveries of practical samples standard addition were 74.2%-95.8%, and the relative standard deviations of the determination results were 1.6%-9.9%(n=6). The method can be used to simultaneously determine of 10 semi-volatile organic compounds in soil.

关 键 词：加压流体萃取 气相色谱-质谱法 苯胺 硝基苯 多环芳烃 土壤 

分 类 号：O657.7[理学—分析化学]