碱解-吹扫捕集气相色谱质谱法间接测定水中三氯杀螨醇  

Indirect determination of dicofol in water by alkaline hydrolysis purge and trap-gas chromatography-mass spectrometry

作　　者：李咏梅 李晨 王惠敏 毛秀丽 张守文[1] LI Yongmei;LI Chen;WANG Huimin;MAO Xiuli;ZHANG Shouwen(Shandong Provincial Lunan Geology and Exploration Institute(Shandong Provincial Bureau of Geology and Mineral Resources No.2 Geological Brigade),Jining 272114,China)

机构地区：[1]山东省鲁南地质工程勘察院(山东省地质矿产勘查开发局第二地质大队),山东济宁272114

出　　处：《化学分析计量》2024年第12期52-57,共6页Chemical Analysis And Meterage

摘　　要：建立了碱解-吹扫捕集气相色谱质谱法间接测定水中三氯杀螨醇的含量。利用三氯杀螨醇在乙醇-氢氧化钠介质下分解为双(对氯苯基)-甲酮和三氯甲烷的特性,通过碱解的手段将三氯杀螨醇分解,然后采用吹扫捕集气相色谱质谱仪测定水中的三氯甲烷,从而间接得出水中三氯杀螨醇的含量。选定的最佳碱解时间为10 min,最佳吹扫时间为11 min。三氯杀螨醇的质量浓度在1~20μg/L范围内与色谱峰面积具有良好的线性关系,相关系数为0.999 4,方法检出限为1.3μg/L,定量限为5.2μg/L。样品的加标回收率为91.7%~98.8%,测定结果的相对标准偏差为4.69%~4.94%(n=6)。该方法可满足测定水中三氯杀螨醇的分析要求。A method for indirect determination of dicofol in water by alkaline hydrolysis-purge and trap-gas chromatography-mass spectrometry was established.The characteristics of dicofol decomposing into bis(2-chlorophenyl)-ketone and trichloromethane in ethanol sodium hydroxide medium was utilized.Triclosan was decomposed by alkaline hydrolysis,and then the trichloromethane in water was measured by purge and trap-gas chromatography-mass spectrometry,indirectly obtaining the content of dicofol in water.The optimal alkaline hydrolysis time was 10 mins,the optimal purging time was 11 minutes.The mass concentration of dicofol had a good linear relationship with the chromatographic peak area in the range of 1-20μg/L,the correlation coefficient was 0.9994.The detection limit of the method was 1.3μg/L,and the quantification limit was 5.2μg/L.The spiked recovery rates of the sample were 91.7%-98.8%,and the relative standard deviations of the measurement results were 4.69%-4.94%(n=6).This method can meet the analytical requirements for determining dicofol in water.

关 键 词：三氯杀螨醇 碱解 吹扫捕集 气质联用仪 水质 

分 类 号：O657.7[理学—分析化学]