【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。更多还原

【Abstract】 A novel method for the determination of 3indicative 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 GC.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 100μL by N2-blowing,13 C12-PCB153 was added as internal standard,and the solution was separated on a DB-5MS column.EI was adopted in MS.The detection limits（3.143S）of P26,P50 and P62were 1,3,5pg,respectively.RSDs（n=5）were all less than 6%.The method was used to determine P26,P50 and P62in a top soil sample,giving results of 0.08,0.04,0.03ng·g^-1,respectively.更多还原