白菜中有机磷农药的电纺纳米纤维固相萃取-高效液相色谱法测定  

Application of Electrospunpolymer Nanofibers in the Determination of Five Organophosphorus Pesticides by HPLC

作　　者：郑春慧[1] 杨立刚[1] 姚志云[1] 赵道远[1] 杨明敏[1] 

机构地区：[1]南京农业大学理学院,江苏南京210095

出　　处：《分析测试学报》2009年第8期926-930,共5页Journal of Instrumental Analysis

基　　金：江苏省高技术研究计划资助项目(BG2007044)

摘　　要：以聚苯乙烯电纺纳米纤维为固相萃取介质填装固相萃取小柱，对白菜中的5种有机磷农药（杀扑磷、马拉硫磷、辛硫磷、丙溴磷、毒死蜱）富集净化，甲醇洗脱吸附在小柱上的农药后，用高效液相色谱-紫外检测器进行检测。对萃取次数、白菜样品提取液、洗脱液、pH值进行了优化，杀扑磷、马拉硫磷、辛硫磷、丙溴磷、毒死蜱在固相萃取小柱上的最大吸附量分别为2．9、3．5、5．6、3．7、7，8mg／g，5种有机磷农药的平均加标回收率为68％～97％，相对标准偏差为1．6％-4．7％。测定喷洒5种农药后的白菜样品的萃取回收率为65％-93％，相对标准偏差为1．6％-4．0％，5种农药的检出限为0．02～0．1mg/kg。该方法操作简单、价廉，能够用于白菜中有机磷农药的测定。A high performance liquid chromatography （HPLC） method was developed for the determination of five organophosphorus pesticides, including methidathion, malathion, phoxim, profenofos and chlorpyrios, in cabbage samples. An electrospunpolymer nanofiber loaded into a tiny tip was used for solid phase extraction materials due to its less fiber amount but large surface areas and strong absorption ability. The five organophosphorus pesticides in cabbage samples was directly extracted with the fiber and eluted by methanol. The detection of the target compounds was performed by LC with UV detector. Experimental parameters influencing the performance of the fiber, such as extracted times, extracted solutions, elutions and pH values were investigated. Under the optimized conditions, the maximum absorption capacities of the fiber for methidathion, malathion, phoxim, profenofos, ehlorpyrios were 2. 9, 3.5, 5.6, 3.7, 7.8 mg/g, respectively. The five organophosphorus pesticides of three concentration standard solutions were extracted by nanofibers, and the extraction recoveries were 68% - 97% with RSDs of 1.6% - 4. 7%. The calibration curves showed good linearity in the concentration range of 0. 05 - 10 mg/L for methidathion, 0. 5 - 10 mg/L for malathion and0. 1 - 10 mg/L for rest of analytes. The limits of detection ranged from 0. 02 to 0. 1 mg/kg for five organophosphorus pesticides. The spiked recoveries were in the range of 65% -93% with RSDs of 1.6% -4.0%. The method was effective, simple and sensitive for detection multiple organophosphorus pesticides. The result also indicated that, compared with usual liquid -liquid extraction and solid phase extraction, the present method offers the advantages of low consumption of organic solvent and less harm to environment and humanity.

关 键 词：电纺纳米纤维 固相萃取 白菜 有机磷 高效液相色谱 

分 类 号：O657.72[理学—分析化学] S482.33[理学—化学]