盐酸黄酮哌酯在碱溶液中的荧光增强反应及其分析应用
发布时间：2019-08-16 06:55
【摘要】：研究了盐酸黄酮哌酯(FX)在强碱溶液中的荧光增强反应,探讨反应机制,建立了药物样品中FX的荧光分析新方法。FX无内源荧光,其强碱水溶液可缓慢产生荧光,加热促进荧光增强反应。FX分解产物的三维荧光图谱中呈现2个荧光峰,激发波长(λex)分别位于223 nm和302 nm,发射波长(λex)均为410 nm。以硫酸奎宁为参比,测得分解产物的荧光量子产率为0.50。FX分解产物的结构表征和光谱解析表明,FX强碱溶液在加热过程中首先发生酯键水解反应,生成3-甲基黄酮-8-羧酸,然后发生γ-吡喃酮环裂解反应,生成α,β-不饱和酮。该产物包含邻羟基苯甲酸结构,在碱性条件下形成分子内氢键,共轭程度增加,刚性增强,因而产生荧光。基于这一荧光增强反应,建立了测定FX的荧光分析方法。在0.020 3~0.487μg·m L-1内,荧光强度与浓度之间的回归方程为IF=23.9+5 357.3 c,r=0.999 7(n=8),检出限D=1.1 ng·m L-1。本法用于盐酸黄酮哌酯片中FX的测定,加标回收率为100.2%,测定结果与紫外分光光度法一致,表明方法可靠。
[Abstract]:The fluorescence enhancement reaction of flavonoids piperate (FX) in strong alkali solution was studied, and the reaction mechanism was discussed. A new method for fluorescence analysis of FX in drug samples was established. FX has no intrinsic fluorescence, its strong alkali aqueous solution can slowly produce fluorescence, heating promotes fluorescence enhancement reaction. There are two fluorescence peaks in the three-dimensional fluorescence spectrum of FX decomposition products, and the excitation wavelength (位 ex) is located at 223 nm and 302 nm, respectively. The emission wavelength (位 ex) is 410 nm.. Using quinine sulfate as reference, the fluorescence quantum yield of the decomposition product was measured as the structure characterization and spectral analysis of 0.50.FX decomposition product. The results showed that the ester bond hydrolysis of FX strong alkali solution occurred first to form 3-methyl flavonoids-8-carboxylic acid, and then gamma-pyranone cyclic cracking reaction to form 伪, 尾-unsaturated ketone. The product contains the structure of o-hydroxybenzoic acid, which forms intramolecular hydrogen bond under alkaline condition, the degree of conjugation increases and the rigidity increases, resulting in fluorescence. Based on this fluorescence enhancement reaction, a fluorescence analysis method for the determination of FX was established. In the range of 0.020 3 ~ 0.487 渭 g 路mL 鈮，
本文编号：2527246
[Abstract]:The fluorescence enhancement reaction of flavonoids piperate (FX) in strong alkali solution was studied, and the reaction mechanism was discussed. A new method for fluorescence analysis of FX in drug samples was established. FX has no intrinsic fluorescence, its strong alkali aqueous solution can slowly produce fluorescence, heating promotes fluorescence enhancement reaction. There are two fluorescence peaks in the three-dimensional fluorescence spectrum of FX decomposition products, and the excitation wavelength (位 ex) is located at 223 nm and 302 nm, respectively. The emission wavelength (位 ex) is 410 nm.. Using quinine sulfate as reference, the fluorescence quantum yield of the decomposition product was measured as the structure characterization and spectral analysis of 0.50.FX decomposition product. The results showed that the ester bond hydrolysis of FX strong alkali solution occurred first to form 3-methyl flavonoids-8-carboxylic acid, and then gamma-pyranone cyclic cracking reaction to form 伪, 尾-unsaturated ketone. The product contains the structure of o-hydroxybenzoic acid, which forms intramolecular hydrogen bond under alkaline condition, the degree of conjugation increases and the rigidity increases, resulting in fluorescence. Based on this fluorescence enhancement reaction, a fluorescence analysis method for the determination of FX was established. In the range of 0.020 3 ~ 0.487 渭 g 路mL 鈮，
本文编号：2527246
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