同位素稀释-气相色谱-高分辨双聚焦磁质谱法测定土壤中毒杀芬的含量  

Determination of Toxaphenes in Soil by High-Resolution Double-Focusing Magnetic MS Combined with Isotope Dilution and GC

作　　者：王荟[1,2] 高占啟[1] 章勇[1,2] 胡冠九[1,2] 

机构地区：[1]江苏省环境监测中心,南京210036 [2]环保部国家地表水有机污染物监测重点实验室,南京210036

出　　处：《理化检验（化学分册）》2016年第1期7-10,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江苏省环境监测科研基金项目(1415)

摘　　要：提出了同位素稀释-气相色谱-高分辨质谱法测定土壤样品中3种指示性毒杀芬Parlar26(P26)、Parlar50(P50)和Parlar62(P62)。以二氯甲烷-丙酮(1+1)混合液为提取溶剂对土壤样品进行微波萃取,提取液经活化硅胶柱净化分离,洗脱液经氮气吹扫浓缩至100μL后,以13C12-PCB153为同位素内标,在DB-5MS色谱柱上分离,质谱中采用电子轰击离子源。P26、P50和P62的检出限(3.143S)分别为1,3,5pg,测定值的相对标准偏差(n=5)小于6%。方法用于某地区表层土壤中3种指示性毒杀芬的检测,测得P26,P50,P62的含量分别为0.08,0.04,0.03ng·g-1。A novel method for the determination of 3 indicative toxaphenes comprised of Parlar26 （P26）. Parlar50 （P50） and Parlar62 （P62） in soil was proposed, based on high-resolution double-focusing magnetic MS combined with isotope dilution and （K2. The sample was treated by microwave assisted extraction with a mixture （1 ＋ 1） of dichloromethane and acetone as solvent. The extract was then purified on an activated silica gel column. The eluate was concentrated to 100 pd. by N2-blowing, 13C12- PCB153 was added as internal standard, and the solution was separated on a DISkSMS column. EI was adopted in MS. The detection limits （3. 143S） of P26, PS0 and P62 were 1, 3, 5 pg, respectively. RSI）s （n=5） were all less than 6%. The method was used to determine P26, P50 and P62 in a top soil sample, giving results of 0. 08,0.04 ,0. 03 ng . g -1 , respectively.

关 键 词：同位素稀释 气相色谱法 双聚焦磁质谱法 毒杀芬 土壤 

分 类 号：O657.63[理学—分析化学]