ASE正交优化-双柱双ECD气相色谱测定土壤中10种硝基苯类化合物和8种有机氯农药  

Determination of 10 nitrobenzene compounds and 8 OCPs in soil by GC coupled with bircolumns and brelectron capture detectors with ASE orthogonal optimization

作　　者：马超云 王钊 谢焱鑫 刘可 李立中 李思阳 Ma Chaoyun;Wang Zhao;Xie Yanxin;Liu Ke;Li Lizhong;Li Siyang(Xiangtan Ecological Environment Monitoring Center of Hunan Province,Xiangtan Hunan 411104,China)

机构地区：[1]湖南省湘潭生态环境监测中心,湘潭411104

出　　处：《分析仪器》2023年第4期29-35,共7页Analytical Instrumentation

摘　　要：基于双柱定性,建立了气相色谱法同时测定土壤中10种硝基苯类化合物和8种有机氯农药分析方法。优化了萃取、净化前处理条件,对比分析了不同进样模式下DDT的降解率。土壤样品在压力为10 MPa、温度为80℃、萃取时间为10 min条件下,经丙酮/正己烷(体积比1:1)混合溶液循环萃取3次后,萃取液过硅酸镁SPE小柱净化,经正己烷/丙酮混合溶液(体积比3:1)洗脱,洗脱液氮吹浓缩至1.0 mL,脉冲进样(压力为10 psi)分析,双柱定性,外标法定量。18种待测物质量浓度在一定范围内与其对应的峰面积呈线性关系,方法检出限(3.143 s)为0.02~0.5μg/kg。按标准加入法对空白样品进行回收试验,回收率在84.0%~116%,测定值的相对标准偏差(n=6)小于等于15.8%;方法用于稻田、蔬菜地、大豆地、茶园4种不同类型土壤样品分析,8种有机氯农药部分检出,含量为1.00~20.9μg/kg。The pretreatment conditions of extraction and purification were optimized,and the DDT degradation rates under different injection modes were compared.Under the conditions of ASE that the pressure was 10 MPa,the temperature was 80℃,and the extraction time was 10 minutes,the soil sample was extracted by acetone/n-hexane(volume ratio 1:1)mixed solution for three times.The extraction liquid was purified by magnesium silicate SPE small column,eluted by n-hexane/acetone mixed solution(volume ratio of 3:1).The elution liquid was concentrated to 1.0 mL by nitrogen blowing,and followed by pulse injection(pressure of 10 psi)analysis,double columns qualitative analysis,and external standard quantitative analysis.Linear relationships between peak area and corresponding mass concentration of 18 substances were in definite ranges,and the detection limit(3.143 s)was in the range of 0.02—0.5μg/Kg.Recovery was tested on the blank sample by standard addition method,the recovery in the range of 84.0%—116%,the RSDs(n=6)was less than or equal to 15.8%.The method was applied to the analysis of four different types of soil samples,including paddy fields,vegetable fields,soybean fields and tea gardens,8 OCPs were partially detected,with concentrations of 1.00—20.9μg/Kg.

关 键 词：ASE正交优化 硝基苯类化合物 有机氯农药 土壤 

分 类 号：O657.71[理学—分析化学] X833[理学—化学]