中空纤维液相微萃取-HPLC法同时测定水样中多种二苯醚类除草剂残留  

Simultaneous determination of multiple biphenyl ether herbicide residues in water samples by hollow fiber liquid-phase microextraction-HPLC method

作　　者：何成艳[1] 黎源倩[2] 孟庆玉[3] 

机构地区：[1]成都中医药大学医学技术学院卫生检验学教研室,成都四川610041 [2]四川大学华西公共卫生学院(华西第四医院) [3]郑州市疾病预防控制中心

出　　处：《现代预防医学》2013年第22期4227-4230,4236,共5页Modern Preventive Medicine

基　　金：卫生部食品卫生标准委员会基金课题(05WSB-01)

摘　　要：目的建立中空纤维液相微萃取-高效液相色谱同时测定水中多种二苯醚类除草剂残留的分析方法。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）的残留经中空纤维膜萃取，采用C18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300nm处测定。采用聚偏氟乙烯中空纤维膜进行液相微萃取，分别优化了影响萃取效率的萃取剂种类、水样pH值、盐浓度、搅拌速度及萃取时间等条件，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0．001-0．20mg／L（苯达松、氟磺胺草醚、三氟羧草醚、苯草醚）、0．001．0．10mg／L（甲羧除草醚、乙羧氟草醚、除草醚、乙氧氟草醚）范围内与其峰面积呈良好的线性关系（r≥0．999），水样的平均加标回收率为78．0％～98．O％，相对标准偏差（RSD）为1．10％～6．90％（n=5）；对于10．0ml水样，本方法的检出限为0．20～0140μg／L。结论本法简便、快速、准确、环境友好、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。OBJECTIVE The study aimed to develop an analytical method for the simultaneous determination of multiple biphenyl ether herbicide residues in water samples by hollow fiber liquid-phase microextraction-HPLC method. METHODS 8 categories of biphenyl ether herbicide residues （bentazone, fomesafen, acifluorfen, aelonifen, bifenox, fluoroglycofen- ethyl, nitrofen, and oxyfluorfen） in water samples were extracted by hollow fiber liquid-phrase microextraction and were gradient-eluted by C 18 chromatography and methanol-triethylamine-hydrochloric acid solution; the residues were detected at 300 nm of wavelength. Polyvinylidene fluoride hollow fiber membrane was used in the liquid-phase microextraction, and extraction efficiency affecting conditions, including type of extractant, pH of water sample, salinity, mixing speed, and extraction time, and chromatographic conditions, including detection wavelength, elution gradient, pH of the mobile phase, flow rate, and column temperature, were optimized. RESULTS Under optimized conditions, mass concentration of the herbicides exhibited a good linear relationship with the peak area at 0.001-0.20 mg/L （for bentazone, fomesafen, acifluorfen, and aclonifen） and 0.001-0.10 mg/L （ for bifenox, fluoroglycofen-ethyl, nitrofen, and oxyiCluorfen） （r t〉 0.999）. Average recovery rate of the water samples ranged between 78.0% and 98.0%, and the relative standard deviation （RSD） was 1.10% -6.90% （n = 5）. For a 10.0 ml water sample, detection limit of the method was 0.2-0.4ug/L. CONCLUSION The method is simple, fast, accurate, environment-friendly, and high in sensitive, and can meet the analytical requirements for the determination of multiple biphenyl ether herbicide residues in envionmental water samples.

关 键 词：液相微萃取 中空纤维膜 高效液相色谱法 二苯醚类除草剂 农药残留分析 水样 

分 类 号：R-331[医药卫生]