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浊点萃取-高效液相色谱法同时测定水中多种二苯醚类除草剂残留
引用本文:何成艳,黎源倩,王慎骄,欧阳华学,郑波.浊点萃取-高效液相色谱法同时测定水中多种二苯醚类除草剂残留[J].四川大学学报(医学版),2010,41(1).
作者姓名:何成艳  黎源倩  王慎骄  欧阳华学  郑波
作者单位:四川大学华西公共卫生学院,卫生检验学教研室,成都,610041
基金项目:卫生部食品卫生标委会基金课题资助 
摘    要:目的 建立同时测定水中多种二苯醚类除草剂残留的浊点萃取-高效液相色谱分析方法.方法 水样中8种二苯醚类除草剂(苯达松、氟磺胺草醚、三氟羧草醚、苯草醚、甲羧除草醚、乙羧氟草醚、除草醚、乙氧氟草醚)的残留经Triton X-114萃取,采用高效液相色谱法,用C_(18)色谱柱分离,以甲醇-三乙胺-盐酸溶液作流动相,梯度洗脱,在波长为300 nm处测定.采用Triton X-114进行浊点萃取,分别优化了影响萃取效率的表面活性剂浓度、水样pH值、盐浓度、平衡温度及时间等条件,并对待测物检测波长、流动相梯度洗脱、流动相pH值、流速和柱温等色谱条件进行了优化.结果 在优化的条件下,待测除草剂的质量浓度在0.05~2.00 mg/L范围内与其峰面积呈良好的线性关系(r=0.9991~0.9998),水样的平均加标回收率,除苯达松较低以外,均在80.1%~100.9%之间,相对标准偏差(RSD)为2.70 OA~6.40%;对于50.0 mL水样,本方法 的检出限为0.10~0.50 μg/L.结论 本法简便、快速、准确、灵敏度高,能满足环境水样中多种二苯醚类除草剂残留分析要求.

关 键 词:浊点萃取  高效液相色谱法  二苯醚类除草剂  农药残留分析  水样

Determination of Biphenyl Ether Herbicides in Water Using HPLC with Cloud-point Extraction
HE Cheng-yan,LI Yuan-qian,WANG Shen-jiao,OUYANG Hua-xue,ZHENG Bo.Determination of Biphenyl Ether Herbicides in Water Using HPLC with Cloud-point Extraction[J].Journal of West China University of Medical Sciences,2010,41(1).
Authors:HE Cheng-yan  LI Yuan-qian  WANG Shen-jiao  OUYANG Hua-xue  ZHENG Bo
Abstract:Objective To determine residues of multiple biphenyl ether herbicides simultaneously in water using high performance liquid chromatography(HPLC)with cloud-point extraction.Methods The residues of eight biphenyl ether herbicides(including bentazone,fomesafen.acifluorfen,aclonifen,bifenox.fluoroglycofenethy,nitrofen,oxyfluorfen)in water samples were extracted with cloud-point extraction of Triton X-114.The analytes were separated and determined using reverse phase HPLC with ultraviolet detector at 300 nm.Optimized conditions for the pretreatment of water samples and the parameters of chromatographic separation applied.Results There was a good linear correlation between the concentration and the peak area of the analytes in the range of 0.05-2.00 mg/L(r=0.9991-0.9998).Except bentazone,the spiked recoveries of the biphenyl ether herbicides in the water samples ranged from 80.1%to 100.9%,with relative standard deviations ranging from 2.70%to 6.40%.The detection limit of the method ranged from 0.10 μg/L to 0.50 μg/L.Conclusion The proposed method is simple,rapid and sensitive,and can meet the requirements of determination of multiple biphenyl ether herbicides simultaneously in natural waters.
Keywords:Cloud point extraction  High performance liquid chromatography  Biphenyl etherherbicides  Multi-residues analysis  Water
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