在线净化加速溶剂萃取–气相色谱–质谱法测定土壤中11种半挥发性有机物  

Determination of 11 semi-volatile organic compounds in soil by accelerated solvent extraction on line purification–GC/MS

作　　者：李婧 耶曼 张利 王岚 LI Jing;YE Man;ZHANG Li;WANG Lan(Xi’an Northwest Geological Institute for Nonferrous Metals Co.,LTD.,Xi’an 710054,China)

机构地区：[1]西安西北有色地质研究院有限公司,西安710054

出　　处：《化学分析计量》2022年第4期73-78,共6页Chemical Analysis And Meterage

摘　　要：采用加速溶剂萃取法对样品进行在线净化和萃取,气相色谱–质谱法测定土壤中11种半挥发性有机物。考察了净化条件、萃取剂、浓缩条件等因素对土壤中11种半挥发性有机物测定的影响,分析了在线净化和离线净化的差异以及在线净化的优势。以弗罗里硅土和石墨化碳黑为净化剂,石英砂为分散剂,土壤样品经快速溶剂萃取仪在线净化萃取,浓缩后采用气相色谱–质谱仪测定。检测结果表明,11种化合物在质量浓度为0.05~2.00 μg/mL范围内与各自的色谱峰面积线性关系良好,平均响应因子的相对标准偏差均小于30%,检出限为0.30~0.65 μg/kg。样品平均加标回收率为85%~105%,相对标准偏差为4.10%~7.05%(n=6)。该方法前处理简便,能够满足土壤中11种半挥发性有机物的同时准确测定。Accelerated solvent extraction and on line purification were used for soil sample treatment,11 semi-volatile organic compounds (SVOCs) in soil were determined by gas chromatography–mass spectrometry(GC–MS).Influence of purification condition,extracting solvent,concentration condition were studied,difference of on line and off line purification as well as superiority of on line purification were also analyzed.Florimetric silica and graphitized carbon black were used as purifying agents,and quartz sand was as dispersing agent,the soil samples were purified and extracted online by rapid solvent extraction apparatus,and then determined by gas chromatography-mass spectrometer after concentration.The mass concentration of 11 SVOCs had a good linear relationship with the chromatographic peak area in their respective ranges of 0.05–2.00 μg/mL,the relative standard deviations of average response factor were less than 30%,and the detection limit of the method was 0.30–0.65 μg/kg.The average spiked recoveries were 85%–105%,and the relative standard deviations of determination results were 4.10%–7.05% (n=6).The method is simple to predispose and could be used for simultaneous and accurate determination of 11 semi-volatile organic compounds in soil.

关 键 词：半挥发性有机物 气相色谱–质谱法 在线净化 土壤 

分 类 号：O657.7[理学—分析化学]