鹽酸黃酮哌酯在堿溶液中的熒光增強(qiáng)反應(yīng)及其分析應(yīng)用
發(fā)布時(shí)間：2019-08-16 06:55
【摘要】：研究了鹽酸黃酮哌酯(FX)在強(qiáng)堿溶液中的熒光增強(qiáng)反應(yīng),探討反應(yīng)機(jī)制,建立了藥物樣品中FX的熒光分析新方法。FX無內(nèi)源熒光,其強(qiáng)堿水溶液可緩慢產(chǎn)生熒光,加熱促進(jìn)熒光增強(qiáng)反應(yīng)。FX分解產(chǎn)物的三維熒光圖譜中呈現(xiàn)2個(gè)熒光峰,激發(fā)波長(zhǎng)(λex)分別位于223 nm和302 nm,發(fā)射波長(zhǎng)(λex)均為410 nm。以硫酸奎寧為參比,測(cè)得分解產(chǎn)物的熒光量子產(chǎn)率為0.50。FX分解產(chǎn)物的結(jié)構(gòu)表征和光譜解析表明,FX強(qiáng)堿溶液在加熱過程中首先發(fā)生酯鍵水解反應(yīng),生成3-甲基黃酮-8-羧酸,然后發(fā)生γ-吡喃酮環(huán)裂解反應(yīng),生成α,β-不飽和酮。該產(chǎn)物包含鄰羥基苯甲酸結(jié)構(gòu),在堿性條件下形成分子內(nèi)氫鍵,共軛程度增加,剛性增強(qiáng),因而產(chǎn)生熒光�；谶@一熒光增強(qiáng)反應(yīng),建立了測(cè)定FX的熒光分析方法。在0.020 3~0.487μg·m L-1內(nèi),熒光強(qiáng)度與濃度之間的回歸方程為IF=23.9+5 357.3 c,r=0.999 7(n=8),檢出限D(zhuǎn)=1.1 ng·m L-1。本法用于鹽酸黃酮哌酯片中FX的測(cè)定,加標(biāo)回收率為100.2%,測(cè)定結(jié)果與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 偽, 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，
本文編號(hào)：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 偽, 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，
本文編號(hào)：2527246
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