高效液相色谱法定量分析金花葵花中5种黄酮类物质  

Simultaneous Determination of Five Flavonoids in the Flowers of Abelmoschus manihot by High Performance Liquid Chromatography

作　　者：吴正超[1] 李亮亮[1] 徐铭泽[1] 臧健[1] WU Zhengchao;LI Liangliang;XU Mingze;ZANG Jian(Shenyang Agricultural University,Shenyang 110866)

机构地区：[1]沈阳农业大学

出　　处：《食品工业》2019年第9期284-287,共4页The Food Industry

基　　金：国家重点研发计划项目(2018YFD0300300)

摘　　要：通过不同提取剂、提取方式、提取条件等对样品前处理条件进行筛选,考察色谱分析条件对分离的影响,建立一种高效液相色谱(HPLC)-二极管阵列检测器(DAD)同时测定金花葵花中5种黄酮类物质(牡荆素鼠李糖苷、牡荆素、芦丁、金丝桃苷、槲皮素)的分析方法。样品以70%甲醇为溶剂,经过30℃超声提取50 min后,离心取上清液,过滤,在流速1.0 mL/min、柱温25℃、进样量20μL条件下,以乙腈-0.05%磷酸溶液为流动相,梯度洗脱,经C18柱(4.6 mm×250 mm, 5μm)分离,采用二极管阵列检测器(DAD),检测波长为355 nm,外标法定量。结果表明,黄酮类待测物在30 min内获得理想的分离。方法的检出限(S/N=3)为8.6~23.6 mg/kg,样品加标浓度在100~20 000mg/kg范围内,平均加标回收率为95.20%~109.48%, RSD (n=6)小于2.24%。该方法检测准确,可实现金花葵花黄酮类成分快速鉴定,为其药效物质基础及质量控制研究提供依据。The sample pretreatment condition was screened by different extracting agents, extraction methods and extraction conditions. The influence of chromatographic condition on separation was investigated. A high performance liquid chromatography(HPLC)-diode array detector(DAD) was established. At the same time, the analytical methods of five flavonoids(vitexin rhamnoside, vitexin, rutin, hyperoside, and quercetin) in the flower sunflower were determined. The sample was extracted with 70% methanol as solvent. After ultrasonic extraction at 30 ℃ for 50 min, the supernatant was centrifuged and filtered. At flow rate of 1.0 mL/min, column temperature of 25 ℃, sample injection volume of 20 μL, acetonitrile-0.05% phosphoric acid solution as mobile phase, gradient elution, the sample was separated by C18 column(4.6 mm×250 mm, 5 μm), and the detection wavelength of diode array detector(DAD) was 355 nm, which was quantified by external standard method. The results showed that the flavonoids were ideally separated within 30 min. The detection limit(S/N=3) of the method was 8.6-23.6 mg/kg, and the spiked concentration of the sample was in the range of 100-20 000 mg/kg. The average spiked recovery was 95.20%-109.48%, and RSD(n=6) was less than 2.24%. The method is accurate and could quickly identify the flavonoids of the flower sunflower flower, which could provide a basis for its pharmacodynamic substance basis and quality control research.

关 键 词：黄酮 超声提取 高效液相色谱 金花葵 

分 类 号：R28[医药卫生—中药学]