Inouye M, Mio T, Sumino K
Department of Public Health, Kobe University School of Medicine, Japan.
Clin Chim Acta. 1987 Dec;170(2-3):305-14. doi: 10.1016/0009-8981(87)90141-0.
A new method for extraction and quantification of plasma o,p'-DDD (2,2-(2-chlorophenyl,4'-chlorophenyl)1,1-dichloroethane) and its metabolites has been developed. When plasma (0.1 ml) adsorbed to and dried on a filter paper was heated with 5% hydrogen chloride in methanol (1 ml) in a boiling water bath, o,p'-DDD and its metabolites were liberated from the serum protein and were able to be easily extracted with benzene. The recovery rate was raised compared with conventional methods. In addition, this procedure also carried out the simultaneous methylation of o,p'-DDA, one of the metabolites. Mass numbers of 199, 210, 235 and 246 were selected from the mass spectra of o,p'-DDD and its related substances, and they were monitored. Identification was performed on the basis of the retention time and the mass peak intensity ratio. Quantitative determination was performed using the internal standard technique. It was learned that o,p'-DDA is present in the plasma at a concentration about 10 times higher than the levels of o,p'-DDD and o,p'-DDE.
已开发出一种提取和定量血浆中邻,对'-滴滴滴(2,2-(2-氯苯基,4'-氯苯基)1,1-二氯乙烷)及其代谢物的新方法。将吸附在滤纸上并干燥的血浆(0.1毫升)与含5%氯化氢的甲醇(1毫升)在沸水浴中加热时,邻,对'-滴滴滴及其代谢物从血清蛋白中释放出来,并能够很容易地用苯萃取。与传统方法相比,回收率有所提高。此外,该程序还对其中一种代谢物邻,对'-滴滴滴乙酸(o,p'-DDA)进行了同时甲基化。从邻,对'-滴滴滴及其相关物质的质谱中选择了199、210、235和246的质量数,并对其进行监测。根据保留时间和质量峰强度比进行鉴定。使用内标技术进行定量测定。据了解,血浆中邻,对'-滴滴滴乙酸的浓度比邻,对'-滴滴滴和邻,对'-滴滴伊(o,p'-DDE)的水平高约10倍。