| 摘要: |
| 建立了固相支撑液液萃取-平行蒸发技术快速净化多种饲料中呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因原药的分析方法，样品采用甲醇-磷酸盐缓冲溶液提取，硅藻土固相支撑液液萃取净化，全自动平行蒸发技术浓缩，高效液相色谱-二极管阵列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。4 种硝基呋喃原药在0.05 ~10 μg/mL范围内线性相关系数大于0.9997，方法定量限为0.1 mg/kg，三个浓度水平0.1、0.2和1.0 mg/kg加标回收率为78.4%~105.3%，相对标准偏差为1.8%~7.2%。饲料实际样品分析结果表明，该方法简化了样品前处理、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。 |
| 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 |
| DOI： |
| 投稿时间：2012-04-18修订日期：2012-06-04 |
| 基金项目:国家质检总局科研项目(2007IK162)与河南省科技攻关项目(122102310456)资助 |
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| Application on a Preparation Method of Solid-supported-liquid-liquid Extraction and Parallel Evaporation for Rapidly Determining Four Nitrofurans Drugs in Feeds |
| 王彩娟 |
| (Henan Entry-exit Inspection and Quarantine Bureau) |
| Abstract: |
| A rapid purification method was established for simultaneous determination of furazolidone, furan ketones, nitrofurazone and nitrofurantoin in feed used solid-supported-liqud-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 on high performance liquid chromatography (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 μg/mL to 10 μg/mL with relative correlations more than 0.9997. The limits of quantification of the method were 0.1 mg/kg. Spiked with 0.1 mg/kg, 0.2 mg/kg and 1 mg/kg, the recoveries were obtained from 78.4% to 105.3% with the relative standard deviation 1.8% to 7.2%. The results of real feeds samples indicated that the method was simple, automatic, accurate, and can be used for quickly quality monitoring analysis of batch feeds. |
| Key words: Nitrofuran solid-supported-liquid-liquid extraction parallel evaporation high performance liquid chromatography |
