摘要
采用超声辅助分散液液微萃取结合气相色谱质谱（DLLME-GC-MS）法,建立海水中5种具有内分泌干扰特性的除草剂（敌草腈、扑灭津、炔苯酰草胺、嗪草酮、氨基丙氟灵）的检测方法。实验考察了萃取剂的种类及用量、分散剂的种类及用量以及萃取溶液的pH和离子强度对萃取效率的影响,最优的DLLME条件为萃取剂氯仿用量为100μL,分散剂乙醇用量为900μL,NaCl浓度为4.0%。结果表明,在最佳的实验条件下,5种除草剂在0.1、0.5、1.0μg/L三个添加水平下,其平均回收率在83.4%-99.6%之间,相对标准偏差为3.1%-10.0%;敌草腈、扑灭津、炔苯酰草胺、嗪草酮、氨基丙氟灵在海水中的检出限分别为0.024、0.010、0.025、0.015、0.030μg/L。该方法具有快速、灵敏、有机溶剂消耗少和重复性好等优点,可用于海水中除草剂类内分泌干扰物的检测。
A method for the simultaneous determination of five herbicides（ dichlobenil,propazine,propyzamide,metribuzin,prodiamine） in seawater samples had been developed by using DLLME coupled with gas chromatography-mass spectrometry（ GC-MS）. The parameters affecting the extraction efficiency in the dispersive liquid-liquid microextraction（ DLLME）,such as types and volumes of dispersive and extraction solvent,the p H and ionic strength of samples,were optimized,being 900μL of ethanol（ dispersive solvent）,100 μL chloroform（ extraction solvent）,4. 0% Na Cl concentration of samples. The average recoveries of three spiked concentrations of 0. 1,0. 5,1. 0 μg / L for five herbicides ranged from 83. 4% to 99. 6%.Limits of determination（ LODs） for dichlobenil,propazine,propyzamide,metribuzin,prodiamine were 0. 024,0. 010,0. 025,0. 015,0. 030 μg / L,respectively. The results demonstrated that the developed method is quick,sensitivity,less consumption of solvent,and has good repeatability. Meanwhile,it could be successfully applied to the analysis of herbicides with the properties of endocrine disrupting in the seawater.
出处
《世界科技研究与发展》
CSCD
2016年第5期1076-1079,1112,共5页
World Sci-Tech R&D
基金
海洋公益性行业专项科研基金(201405035)
宁波大学学科基金(xkzsc1412)
宁波市科技计划(2014C10063)资助
