人血清中666、DDT气相色谱测定方法的研究  

STUDY ON THE DETERMINATION OF 666,DDT IN HUMAN SERUM BY GAS CHROMATOGRAPHY

作　　者：曾红燕[1] 黎源倩[1] 邹晓莉[1] 陈路齐[1] 

机构地区：[1]四川大学华西公共卫生学院,成都610041

出　　处：《现代预防医学》2007年第3期407-411,共5页Modern Preventive Medicine

基　　金：国家自然科学基金重点项目(30030120)资助

摘　　要：[目的]建立人血清中666、DDT的检测方法,为研究它们与乳腺癌之间的关系提供灵敏、可靠的实验依据。[方法]用正己烷超声波提取人血清样品中666和DDT,磺化处理后,用气相色谱法,电子捕获检测器测定。[结果]采用气相色谱-电子捕获检测器(GC-ECD)测定人血清中4种666和4种DDT有机氯农药含量,日内精密度在2.16%～6.83%范围内,日间精密度为2.50%～7.40%,加标回收率在89.9%～102.0%之间。α-666、γ-666、σ-666及p,p'-DDE在0.0002～0.50 μg/ml范围内线性良好,β-666和p,p'-DDD的线性范围在0.0004～0.50 μg/ml之间,o,p'-DDT和p,p'-DDT的线性范围分别为0.0007～0.50 μg/ml和0.001～0.50 μg/ml。线性相关系数均在0.99以上,检出限0.07～0.52 ng/ml。[结论]建立了人血清中有机氯GC-ECD测定方法,对52例对照及15例乳腺癌病例的人血清进行了测定。病例组血清中8种有机氯的均值有7种高于对照组。病例组中p,p,-DDT、o,p,-DDT和p,p,-DDE的均值和检出率均比对照组高,且用SPSS软件分析后显示差异具有统计学意义(P﹤0.05),提示DDT可能是乳腺癌发病的相关因素。[Objective] To develop a sensitive and reliable analytical method for the study of the relationship between organochloride pesticides （666 and DDT） and mammary cancer. [Methods] 666 and DDT in hnman serum were extracted ultrasonically with hexane, cleaned up with concentrated sulfuric acid, concentrated and determined by gas chromatography with ECD. [Results] Four isomers of 666 and four isomers of DDT in human serum were determined by GC-ECD. The withinday precisions were 2.16%- 6.83%, the between-day precisions were 2.50%-7.40%. The recoveries for the spiked samples ranged from 89.9% to 102.0%. Under these conditions, 666 and DDT were well seperated and showed good linearity in the studies ranges （0.000 2-0.50 μg/ml for α-BHC, γ-BHC, δ-BHC and p, p＇-DDE, 0.000 4-0.50 μg/ml for β-BHC and o, p＇-DDD, 0.000 7-0.50 μg/ml for o, p＇-DDT and 0.001-0.50 μg/ml for p, p＇-DDT） with correlation coefficients greater than 0.99. The detection limits of the method were 0.07-0.52 ng/ml. [Conclusions] The GC-ECD method has been applied to determine organochloride pesticides in human serum. Analytes have been determined in 52 control serum samples and 15 mammary cancer serum samples. The mean concentrations of seven of eight isomers are greater in case group than those in control group and there is a significant difference for p, p, -DDT, p, p, -DDE and o, p, -DDT in deteeable rate between case group and control group, respectively, assessed by SPSS with P 〈 0.05. This indicates that these substances may be related factors of occurrence of mammary cancer.

关 键 词：气相色谱法 有机氯农药 666 DDT 人血清 

分 类 号：O657.71[理学—分析化学]