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作 者:马红燕[1] 罗娟娟[1] 杨猛[1] 梁金榜[1]
机构地区:[1]延安大学化学与化工学院分析化学研究所,延安716000
出 处:《分析试验室》2011年第5期42-45,共4页Chinese Journal of Analysis Laboratory
基 金:陕西省教育厅专项科研基金资助课题(09JK821);延安市科技局科技计划项目(2008ks-20)资助
摘 要:研究了美洛昔康-Ce(Ⅳ)-β-环糊精(β-CD)体系的荧光特性。实验发现,美洛昔康自身几乎没有荧光,但其能使Ce(1V)定量还原为Ce(Ⅲ),Ce(Ⅲ)能发射特征荧光,β-CD的加入对体系的荧光强度有增敏增稳作用,基于在λex=260nm和λem=362nm处测定Ce(Ⅲ)的荧光强度,提出了β-CD增敏间接荧光光谱法测定微量美洛昔康的新方法。方法线性范围为8.0×10^-10~3.2×10^-7g/mL,检出限为3.5×10^-10/mL,相对标准偏差为2.0%(n,=5,c=4.0×10^-8g/mL)。方法用于片剂和尿样中美洛昔康的分析测定。A novel and sensitive spectrofluorimetric method for the determination of meloxicam has been developed. The experiments indicated that meloxicam has little fluorescence signal by itself, but it could reduce cerium (IV) to cerium ( Ⅲ ). Cerium (Ⅲ ) could emit characteristic fluorescence at λce= 260 nm and λem = 362 nm in sulfuric acid medium. When ,β-cyclodextrin (β-CD) was added into the system, the fluorescenceintensity could be enhanced greatly. Based on this meloxicam-cerium ( IV)-β-CD fluorescence system, a new fluorescent method was established for the indirect determination of meloxicam. The experimental conditions that influenced the fluorescence intensity, such as : the reaction medium and pH, the concentration of cerium (IV) , the influence of surfactants and β-CD, the concentration of β-cyclodextrin and stability, et al were investigated and optimized. Under optimal experimental conditions, the linear range was 8.0× 10^-10- 3.2 x 10^-7g,/mL, the detection limit was 3.5 x 10^-10g/mL, and the relative standard derivation was 2.0% (n = 5, c = 4.0 x 10^-8 g/mL). It has been used for the determination of meloxicam in tablets and human urines.
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