色谱

色谱 ›› 2014, Vol. 32 ›› Issue (4): 402-406.DOI: 10.3724/SP.J.1123.2013.10013

• 庆祝《色谱》创刊三十周年暨卢佩章院士九十华诞专刊-研究论文 • 上一篇    下一篇

基于整体材料搅拌棒固相萃取高效液相色谱联用测定饲料和水样中硝基呋喃类药物残留

张咏, 梅萌, 黄晓佳, 袁东星   

  1. 厦门大学环境与生态学院 滨海湿地生态系统教育部重点实验室, 福建 厦门 361005
  • 收稿日期:2013-10-16 修回日期:2013-12-17 出版日期:2014-04-08 发布日期:2014-03-28
  • 通讯作者: 黄晓佳
  • 基金资助:

    国家自然科学基金项目（21377105，21077085）；福建省新世纪优秀人才项目.

Determination of nitrofuran residues in feed and water samples by monolith-based stir bar sorptive extraction and high performance liquid chromatography

ZHANG Yong, MEI Meng, HUANG Xiaojia, YUAN Dongxing   

  1. Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China
  • Received:2013-10-16 Revised:2013-12-17 Online:2014-04-08 Published:2014-03-28

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摘要：

利用自制的以聚（乙烯基咪唑-二乙烯基苯）（VIDB）整体材料为涂层的固相萃取搅拌棒（VIDB-SBSE）萃取3种硝基呋喃类药物，然后与高效液相色谱-二极管阵列检测器联用建立了测定饲料和水样品中硝基呋喃类药物残留的方法。详细考察了萃取过程中萃取和解吸时间、样品基质的pH值以及离子强度等实验条件对萃取效率的影响。在最佳条件下，呋喃唑酮的线性范围为0.5~200 μg/L，呋喃妥因和呋喃西林的线性范围为0.25~200 μg/L，3种目标物的检出限（LOD）（S/N=3）在0.068~0.11 μg/L之间，所建方法具有理想的日内和日间重现性（RSD值均小于6%）。在对饲料和实际水样的测定中，不同加标浓度呋喃唑酮、呋喃妥因和呋喃西林的回收率在80.6%~108%之间。研究表明，所建立的方法具有简便、灵敏、环境友好等特点。

关键词: 高效液相色谱, 搅拌棒吸附萃取, 水样, 饲料, 硝基呋喃类残留, 整体材料

Abstract:

A simple, efficient and sensitive method for the simultaneous determination of nitrofurantoin (NFT), furazolidone (FZD) and nitrofurazone (NFZ) in feed and water samples was developed by stir bar sorptive extraction (SBSE) coupled to high performance liquid chromatography with diode array detection. The SBSE based on poly (vinylimidazole-divinylbenzene) (VIDB) monolithic material as coating was used to concentrate the three target analytes. To obtain the optimum extraction performance, several VIDB-SBSE parameters were investigated and studied, including pH value, ionic strength of sample matrix, extraction and desorption time. Under the optimized experimental conditions, the linear ranges were 0.5-200 μg/L for FZD, 0.25-200 μg/L for NFT and NFZ. The limits of detection (S/N=3) were in the range of 0.068-0.11 μg/L for the three analytes. The precision of the proposed method was evaluated in terms of intra- and inter-day repeatability calculated as RSD, and it was found that the RSDs were all below 6%. The developed method was successfully applied to the determination of nitrofuran residues in animal feed and water samples. The satisfactory recoveries of the spiked target compounds were in the range of 80.6%-108%.

Key words: feed, high performance liquid chromatography (HPLC), monolithic material, nitrofuran residues, stir bar sorptive extraction (SBSE), water samples

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