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胶束增敏和铽敏分子印迹固相萃取分光光度法测定牛奶中的丹氟沙星

Micelle enhanced and terbium sensitized spectrofluorimetric determination of danofloxacin in milk using molecularly imprinted solid phase extraction.

机构信息

Department of Chemistry, Punjabi University, Patiala 147 002, Punjab, India.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2012 Oct;96:790-5. doi: 10.1016/j.saa.2012.07.083. Epub 2012 Aug 3.

Abstract

An efficient molecularly imprinted solid phase extraction (MISPE)-spectrofluorimetric method was developed to sensitively determine danofloxacin (DAN) in milk samples. Solid phase extraction procedure using MISPE cartridges was first performed on milk samples and then spectrofluorimetric determination was done at 546 nm using an excitation wavelength of 285 nm in presence of terbium and sodium dodecyl benzene sulfonate (SDBS). It was found that SDBS significantly enhanced the fluorescence intensity of the DAN-Tb(3+) complex. Various factors affecting the fluorescence intensity of DAN-Tb(3+)-SDBS system were studied and conditions were optimized. The enhanced fluorescence intensity of the system (ΔF) showed a good linear relationship with the concentration of DAN over the range of 8.4×10(-9)-3.4×10(-7) mol L(-1) with a correlation coefficient of 0.9996. The detection limit was determined as 2.0×10(-9) mol L(-1) and the limit of quantification was determined as 6.5×10(-9) mol L(-1). The MISPE-spectrofluorimetric procedure was successfully applied to the determination of DAN in milk samples. The method is simple, rapid, sensitive and allows interference free determination of DAN in complex fluorescent matrices like milk. The method can be used to determine whether the DAN residues in milk exceed MRLs or not.

摘要

建立了一种高效的分子印迹固相萃取(MISPE)-荧光光谱法,用于灵敏测定牛奶样品中的丹诺沙星(DAN)。首先通过 MISPE 小柱对牛奶样品进行固相萃取处理,然后在 285nm 激发波长下,于存在铽和十二烷基苯磺酸钠(SDBS)时,在 546nm 处进行荧光光谱测定。结果表明,SDBS 显著增强了 DAN-Tb(3+)配合物的荧光强度。研究了影响 DAN-Tb(3+)-SDBS 体系荧光强度的各种因素,并对条件进行了优化。该体系的增强荧光强度(ΔF)在 8.4×10(-9)-3.4×10(-7) mol L(-1)范围内与 DAN 的浓度呈良好的线性关系,相关系数为 0.9996。检测限确定为 2.0×10(-9) mol L(-1),定量限确定为 6.5×10(-9) mol L(-1)。该 MISPE-荧光光谱法成功应用于牛奶样品中 DAN 的测定。该方法简单、快速、灵敏,可在牛奶等复杂荧光基质中进行无干扰的 DAN 测定。该方法可用于判断牛奶中的 DAN 残留是否超过 MRLs。

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