Zencak Zdenek, Reth Margot, Oehme Michael
Organic Analytical Chemistry, University of Basel, Neuhausstrasse 31, 4057 Basel, Switzerland.
Anal Chem. 2003 May 15;75(10):2487-92. doi: 10.1021/ac034090c.
The use of dichloromethane/methane reagent gas mixtures is described as an alternative to conventional electron capture negative ionization for the determination of polychlorinated n-alkanes (PCAs). A nearly exclusive formation of [M + Cl]- adduct ions was observed suppressing the generation of other fragment ions. The resulting enhanced selectivity and sensitivity lowered quantification limits to 3 ng for a technical PCA mixture and 10.5-13.5 pg for single congeners. Response factors for congeners of different degrees of chlorination varied by not more than a factor of 2. Interferences from other polychlorinated compounds present in environmental samples such as toxaphene or chlordanes were suppressed by a factor of 5 or more. The technique was applied for the determination of the composition of technical PCA mixtures as well as for the analysis of PCAs in North Sea dab liver.
二氯甲烷/甲烷反应气混合物的使用被描述为一种用于测定多氯正构烷烃(PCA)的传统电子捕获负电离的替代方法。观察到几乎只形成[M + Cl]-加合离子,抑制了其他碎片离子的产生。由此提高的选择性和灵敏度将技术PCA混合物的定量限降低到3 ng,单个同系物的定量限降低到10.5 - 13.5 pg。不同氯化程度同系物的响应因子变化不超过2倍。环境样品中存在的其他多氯化合物(如毒杀芬或氯丹)的干扰被抑制了5倍或更多。该技术用于测定技术PCA混合物的组成以及分析北海鲽鱼肝脏中的PCA。