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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 被引量:1

Determination of Toxaphenes in Soil by High-Resolution Double-Focusing Magnetic MS Combined with Isotope Dilution and GC
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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.
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 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)
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 Isotope dilution GC High-resolution double-focusing magnetic MS Toxaphene Soil
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