三氯杀螨醇在气相色谱系统中的降解研究  

Investigation on Degradation of Dicofol in Gas Chromatography System

作　　者：钱振杰 王宇 赵金利 王成龙 黄松 谭锦萍 黄小清 林泽珊 刘佳 QIAN Zhen-jie;WANG Yu;ZHAO Jin-li;WANG Cheng-long;HUANG Song;TAN Jin-ping;HUANG Xiao-qing;LIN Ze-shan;LIU Jia(Guangzhou Food Inspection Institute,Guangzhou 511400,China)

机构地区：[1]广州市食品检验所,广东广州511400

出　　处：《分析测试学报》2022年第12期1765-1772,共8页Journal of Instrumental Analysis

基　　金：广州市市场监督管理局科技项目(2021KJ48)。

摘　　要：采用气相色谱系统,识别和推测了三氯杀螨醇的主要降解产物及其结构,研究了其在进样口和有机溶剂中的降解行为,并提出了解决降解影响的措施。结果表明,三氯杀螨醇主要的降解产物除4,4’-二氯二苯甲酮(4,4’-DBP)外,还存在一种通过脱氯途径生成的降解物。当进样口温度低于260℃时,三氯杀螨醇基本保持稳定;三氯杀螨醇在甲苯中的稳定性较好,在丙酮和乙腈中则完全降解成4,4’-DBP,而对溶剂脱水可减缓该反应的发生;在乙酸乙酯中三氯杀螨醇通过脱氯途径部分降解,在溶剂中添加卤代物可抑制该反应的发生。由于样品基质极性的不确定性,最终选取三氯杀螨醇、4,4’-DBP及脱氯降解物为标志物,以三者峰面积加和的方式对样品中三氯杀螨醇的残留量进行定量分析。采用该方法测得油麦菜、苹果和红茶3种不同基质在0.01、0.05、0.1 mg/kg加标水平下的平均回收率为72.5%~110%,相对标准偏差(RSD,n=6)为5.1%~10%。该研究为三氯杀螨醇的准确定性和定量测定提供了实验依据,并对探索同类结构化合物的降解行为具有参考价值。Gas chromatography system was utilized to identify the main degradation products and structures of dicofol.Its degradation behaviors in the inlet and organic solvents were investigatied and the measures to minimize the degradation effects on the analysis were proposed.The results showed that the main degradation products of dicofol,in addition to the reported 4,4’-DBP,were obtained through the de-chlorination pathway.Generally,dicofol is stable when the inlet temperature is lower than 260 ℃,and it is stable in toluene but completely degrade to 4,4’-DBP in acetone and acetonitrile.Meanwhule,anhydrous solvent could slow down the degradation process.In ethyl acetate,dicofol could be partly degraded by dechlorination.The addition of halides to the solvent could prohibit the dechlorination.Dicofol,4,4’-DBP and degraded products were used to determine the residual amount of dicofol in the actual sample matrix by measuring the sum of the three peak areas due to the uncertainty of the sample matrix polarity.The average recoveries of this method for three matrixes at 0.01,0.05 and 0.1 mg/kg spiked levels ranged from 72.5% to 110%,with the relative standard deviations(RSDs,n = 6)of 5.1%-10%.This study provides an experimental basis for accurate,qualitative and quantitative detection of dicofol,which is of a certain reference value for exploring the degradation of compounds with the smilar structure.

关 键 词：三氯杀螨醇 降解 进样口温度 溶剂 定量 气相色谱系统 

分 类 号：O657.7[理学—分析化学] S482.32[理学—化学]