摘要
建立并优化了土壤中三甲基铅(TML)和三乙基铅(TEL)形态提取方法,构建了高效液相色谱-电感耦合等离子体质谱联用技术分离测定三甲基铅(TML)和三乙基铅(TEL)形态的分析方法。通过改变流动相组分比例,使TML和TEL的有机铅形态达到基线分离。TML和TEL有机铅的检出限分别达到0.15μg·kg-1和0.35μg·kg-1;峰面积的RSD分别为4.6%和5.5%。对浓度范围为0.5~100μg·kg^(-1)有机铅混合标准溶液进行线性动态范围测定,结果两种有机铅的回归系数均在0.9998以上。比较了几种不同的样品提取方法,得到土壤用80%甲醇的乙酸溶液振荡过夜后,上清液pH调值至9,用0.5mol·L^(-1)的DDTC、0.1mol·L^(-1)的EDTA和正己烷溶液提取,TML和TEL的加标回收率均大于98.0%。利用建立的方法,对实际土壤样品进行有机铅测定,在部分样品中检测到TML和TEL有机铅化合物形态。
A method for the speciation analysis of organoleads compounds including Trimethyllead(TML)and Triethyllead(TEL)was established using high performance liquid chromatography-inductively coupled plasma-mass spectrometry(HPLC-ICP-MS).Besides,an extraction method for the TML and TEL in soil was developed and optimized.After evaluation of different additives in the mobile phase,the use of methanol! water(30∶70)allowed the best chromatographic separation of the two compounds.The method detection limit for TML and TEL were 0.15μg·kg^(-1) and 0.35μg·kg^(-1) respectively,and the RSD of their Peak area were 4.6%,and 5.5%.Two mixed organolead standards from 0.5μg·kg^(-1) to 100μg·kg^(-1) was used for the method evaluation.The experimental results indicate that the regression coefficient for each compound was over 0.9998.The type and volume of organic extraction solvent,pH,effect of added salt content,and centrifuging time and speed were investigated.Under the optimum extraction conditions,the analytes were extracted into a extractant reagent(V(methanol)∶V(water)=80∶20%)by mechanically shaken overnight,and extracted by 0.5 mol·L^(-1) DDTC,0.1 mol·L^(-1) EDTA and hexane.The recoveries for TML and TEL in soil were over 98.0%.Organolead compounds in soil samples were analyzed via the new established method.TML and TEL were detected in some soil samples.
出处
《化学研究与应用》
CSCD
北大核心
2017年第11期1641-1646,共6页
Chemical Research and Application
基金
中国地质科学院基本科研业务费项目(YYWF201620)资助
关键词
HPLC-ICP-MS
振荡提取
三甲基铅
三乙基铅
土壤
high performance liquid chromatography-inductively coupled plasma mass spectrometry
shake extraction
trimethyllead
triethyllead
soil
