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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Determination of piceid by photochemically induced fluorescence and second-derivative - Response surface methodology for the optimization of a liquid-liquid extraction procedure for its analysis in wine samples
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Determination of piceid by photochemically induced fluorescence and second-derivative - Response surface methodology for the optimization of a liquid-liquid extraction procedure for its analysis in wine samples

机译:光化学诱导荧光和二阶导数-响应面法测定酒中的类固醇,优化酒液中液-液萃取程序的分析

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trans-Piceid itself is weakly fluorescent, but the fluorescence signal (lambda(exc/em) = 260/361 nm) is greatly enhanced by UV-irradiation of its hydroethanolic solutions. Employing the photoinduced emission signal at 361 nm or the amplitude of the second-derivative-photoinduced emission spectrum, between 353 and 361 nm, a linear relation is found in the assayed range 5.7-31.4 ng mL(-1) of trans-piceid and limits of detection of 1.7 and 2.1 ng mL(-1), respectively, are obtained. A previous liquid-liquid extraction is necessary for the determination of piceid in wine. Experimental design (Central Composite Design) together with the Response Surface Methodology have been used to find optimum conditions for the extraction procedure. For this purpose, the difference between the photoinduced-fluorescence signal = (lambda(exc/em) = 260/361 nm) of the aqueous phase, before and after being extracted, has been considered as Response Function. A tartrate buffer (pH 5.0) concentration of 0.15 mol L-1 and a phase ratio of 1 are determined as optimum conditions. The amplitude of the second-derivative-emission spectrum, corresponding to the evaporated and re-dissolved organic phase, between 353 and 361 nm has been employed as analytical signal. Standard addition method has been applied to the analysis of piceid in different wine samples under optimum conditions. Results of wine analysis have been satisfactorily validated by HPLC. (c) 2007 Elsevier B.V. All rights reserved.
机译:反式皮卡西德本身的荧光很弱,但是通过对其氢乙醇溶液进行紫外线照射,荧光信号(λ(exc / em)= 260/361 nm)大大增强了。利用361 nm处的光致发射信号或353至361 nm之间的二阶光导光致发射光谱的幅度,发现在经测定的5.7-31.4 ng mL(-1)范围内,反式-双萜和分别获得了1.7和2.1 ng mL(-1)的检出限。为了确定葡萄酒中的杀虫剂,必须先进行液-液萃取。实验设计(中央复合设计)与响应面方法一起用于寻找提取程序的最佳条件。为此,在提取之前和之后,水相的光致荧光信号=(λ(exc / em)= 260/361 nm)之间的差异被视为响应函数。确定酒石酸缓冲液(pH 5.0)浓度为0.15 mol L-1和相比为1是最佳条件。对应于蒸发和重新溶解的有机相的二阶导数发射光谱的振幅在353和361 nm之间已被用作分析信号。在最佳条件下,标准添加方法已用于分析不同葡萄酒样品中的仿生菌。葡萄酒分析的结果已通过HPLC令人满意地验证。 (c)2007 Elsevier B.V.保留所有权利。

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