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采用反相分散液液微萃取结合高效液相色谱-紫外检测法,建立了一种灵敏、高效的测定蜂蜜和生物样品中槲皮素的方法。

Utilization of inverted dispersive liquid-liquid microextraction followed by HPLC-UV as a sensitive and efficient method for the extraction and determination of quercetin in honey and biological samples.

机构信息

Department of Analytical Chemistry, Faculty of Chemistry, University of Mazandaran, Babolsar, Iran.

出版信息

Talanta. 2012 Jan 30;89:117-23. doi: 10.1016/j.talanta.2011.11.079. Epub 2011 Dec 4.

Abstract

A sensitive, rapid and efficient method for the extraction of quercetin as well as its determination in honey and biological samples was developed using inverted dispersive liquid-liquid microextraction (IDLLME) and HPLC-UV. The extraction method is based on the application of an extracting solvent lighter than water in the ternary component solvent (aqueous solution: extracting solvent: disperser solvent) system. The extraction parameters such as type and volume of extracting and disperser solvent, pH of sample, stirring rate and extraction time were optimized. Under the optimal conditions (extracting solvent: 100 μL 1-octanol; disperser solvent: 300 μL acetonitrile; pH of sample: 4.5 and stirring rate: 1000 rpm) a linear calibration curve was obtained in the range of 0.5-1000 ng mL(-1) with R(2)=0.9993 (n=10). The limits of detection and quantification were 0.26 and 0.78 ng mL(-1), respectively. The extraction recovery was 97% and the preconcentration factor was 243. While the relative standard deviation for 25 ng mL(-1) was 3.51 (n=5), it was 2.12 (n=5) for 500 ng mL(-1) of quercetin. The method was successfully applied for the preconcentration and determination of quercetin in honey, urine and plasma samples.

摘要

建立了一种灵敏、快速、高效的提取槲皮素的方法,并采用反相分散液液微萃取(IDLLME)和高效液相色谱-紫外检测法(HPLC-UV)对其进行了测定。该提取方法基于在三元溶剂(水相:萃取溶剂:分散溶剂)体系中使用比水轻的萃取溶剂。优化了提取参数,如萃取溶剂和分散溶剂的类型和体积、样品 pH 值、搅拌速度和提取时间。在最佳条件下(萃取溶剂:100 μL 正辛醇;分散溶剂:300 μL 乙腈;样品 pH 值:4.5,搅拌速度:1000 rpm),在 0.5-1000 ng mL(-1) 范围内得到了线性校准曲线,R(2)=0.9993(n=10)。检测限和定量限分别为 0.26 和 0.78 ng mL(-1)。萃取回收率为 97%,浓缩因子为 243。当槲皮素浓度为 25 ng mL(-1) 时,相对标准偏差为 3.51(n=5),当浓度为 500 ng mL(-1) 时,相对标准偏差为 2.12(n=5)。该方法成功应用于蜂蜜、尿液和血浆样品中槲皮素的预浓缩和测定。

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