加速溶剂萃取-丙基化衍生-气相色谱质谱法测定土壤中的三甲基铅与三乙基铅  

Detection of trimethyl lead and triethyl lead in soil by ASE-GC-MS with sodium tetrapropylborate as derivatization reagent

作　　者：孙蕊蕊 王馨蕾 张守文[2] 朱艳艳 崔兆杰[1] SUN Rui-rui;WANG Xin-lei;ZHANG Shou-wen;ZHU Yan-yan;CUI Zhao-jie(School of Environmental Science and Engineering,Shandong University,Qingdao 266000;Lunan Geo-engineering Exploration Institute of Shandong Province,Jining 272000)

机构地区：[1]山东大学环境科学与工程学院,青岛266000 [2]山东省鲁南地质工程勘察院实验测试中心,济宁272000

出　　处：《分析试验室》2019年第12期1490-1494,共5页Chinese Journal of Analysis Laboratory

基　　金：济钢污染场地重金属-有机物复合污染联合修复机理及风险评估项目(ZR2018ZC2362)资助

摘　　要：建立了加速溶剂萃取-丙基化衍生-气相色谱质谱联用分析土壤中的三甲基铅与三乙基铅的方法。不加任何填充物,温度为100℃,静态萃取时间5 min,循环次数为2次,冲洗体积为65%,吹扫时间90 s时得到最大的回收率;在此条件下,三甲基铅与三乙基铅的的回收率分别为92.12%,90.54%。三甲基铅与三乙基铅在0.05~20 mg/L的范围内,具有良好的线性关系(r 2≥0.999),其方法检出限分别为0.02 mg/kg及0.025 mg/kg。将该方法应用于真实样品的检测,样品加标回收率可达90%以上,相对标准偏差(RSD)小于6%。适用于土壤中三甲基铅与三乙基铅的分析。A method for the determination of trimethyl lead(TML)and triethyl lead(TEL)in soil was developed using accelerated solvent extraction(ASE)followed by gas chromatography-mass spectrometry.The factors influencing the extraction efficiency of ASE were investigated,and the optimum extraction conditions were as follow:no filler,temperature of 100℃,static time of 5 min,2 cycles,65%flush volume,purge time of 90 s.The recoveries of TML and TEL were 92.12%and 90.54%under the optimal extraction condition,respectively.Favourable linear relationships of TML and TEL were obtained in the range of 0.05-20 mg/L with satisfied correlation coefficients(r 2≥0.999),and the limits of quantitation(LOQ)were 0.02 and 0.025 mg/kg respectively.This method was further employed in the actual sample assays with the spiked recovery above 90%and the RSD below 6%.The method can be used to analyzed organolead in soil.

关 键 词：加速溶剂萃取 三甲基铅 三乙基铅 四丙基硼化钠 气相色谱质谱法 

分 类 号：O657.63[理学—分析化学]