应用固相支撑液液萃取-平行蒸发前处理技术检测饲料中四种硝基呋喃类药物  

Application of Solid-supported-liquid-liquid Extraction and Parallel Evaporation for Determination of Four Nitrofurans Drugs in Feeds

作　　者：王彩娟[1,2] 祝伟霞 杨冀州 孙转莲 张巨洲 张书胜[2] 

机构地区：[1]河南出入境检验检疫局,郑州450003 [2]郑州大学化学与分子工程学院,郑州450042

出　　处：《中国兽药杂志》2012年第12期36-39,共4页Chinese Journal of Veterinary Drug

基　　金：国家质检总局科研项目(2007IK162);河南省科技攻关项目(122102310456)

摘　　要：建立了固相支撑液液萃取-平行蒸发技术用于快速净化多种饲料中的呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因。先用甲醇-磷酸盐缓冲溶液提取样品,再用硅藻土固相支撑液液萃取净化,然后用全自动平行蒸发技术浓缩,最后用高效液相色谱-二极管阵列在365 nm波长下检测。实验对提取溶剂、净化方法、萃取时间、萃取体积和色谱分离等实验条件进行了优化。四种硝基呋喃原药在0.05～10μg/mL范围内线性相关系数大于0.9997,方法定量限为0.1 mg/kg,0.1、0.2、1.0 mg/kg三个浓度水平的加标回收率为78.4%～105.3%,相对标准偏差为1.8%～7.2%。实际饲料样品分析结果表明,该技术简化了样品前处理,提高了操作自动化程度,测定结果准确度高,可用于批量饲料样品中硝基呋喃类原药的快速质量监控分析。A rapid purification method was established for simultaneous determination of furazolidone, furan ketones, nitrofurazone and nitrofurantoin in feed using solid - supported - liquid - liquid extraction and parallel evaporation. The samples were extracted with methanol -phosphate buffer. The purification procedure was used with solid- supported- liquid- liquid extraction （SSLLE） and the concentration was selected with an automatic method of parallel evaporation （PE）. The detection was performed by HPLC with diode - array detector （DAD） under 365 nm. The experimental parameters including extraction solvent, purification, extract time, extraction volumes, separation conditions were optimized. With the optimal conditions, the linear range of analytes was from 0.05 to 10 txg/mL with relative correlations more than 0.9997. The limit of quantification of the method was 0.1mg/kg. Spiked with 0.1,0.2 and 1 mg/kg, the recoveries were obtained from 78.4% to 105.3% with the relative standard deviation from 1.8% to 7.2%. The results of real feeds samples indicated that the method was simple, automatic, accurate, and can be used for quick quality monitoring analysis of batch feeds.

关 键 词：硝基呋喃 固相支撑液液萃取 平行蒸发 高效液相色谱 

分 类 号：S859.83[农业科学—临床兽医学]