摘要
通过静态吸附研究了七种大孔吸附树脂对西南委陵菜黄酮的纯化效果,利用动态吸附考察了样品液的吸附流速和pH值、解吸剂pH值和乙醇浓度等影响因素。发现大孔吸附树脂D101对西南委陵菜黄酮的纯化效果最佳,最佳条件为:样品液pH 4、吸附流速2 BV/h、解吸剂pH 8、解吸剂中乙醇浓度为60%,使纯度由28.24%提高到46.60%。利用高效液相色谱电喷雾离子化串联二级质谱(HPLC-ESI-MS/MS),根据保留时间、分子离子、二级质谱碎片,对西南委陵菜黄酮成分进行定性分析。通过多反应监控模式(MRM)监控特定碎片离子,以及三种标准品的标准曲线,分别利用外标法和内标法对黄酮进行了定量分析。西南委陵菜黄酮的主要成分及其含量为:芹黄素-7-O-β-D-葡糖苷酸(6.66μg/mg)、金丝桃苷(2.39μg/mg)、紫云英苷(2.30μg/mg)、野黄芩苷(1.95μg/mg)、木犀草苷(0.44μg/mg)、翻白叶苷A(0.39μg/mg)和异牡荆素(0.01μg/mg)。
Purification effects of seven kinds of macroporous resins through static adsorption on the flavonoids from Potentilla fulgens were studied. The factors including the flow rate, pH of the sample solution, ethanol concentration and pH of the desorbent were determined through dynamic adsorption. The results showed that macroporous resin D101 was the best to purify flavonoids from Potentilla fulgens. The optimal purifying conditions were as follows： the adsorption flow rate 2 BV/h, sample solution pH 4, desorbent pH 8, and 60% ethanol in the desorbent and the purity of flavonoids increased from 28.24% to 46.60%. The flavonoids were qualitatively identified using high performance liquid chromatography-electrospray tandem mass spectrometry （HPLC-ESI-MS/MS）, according to retention time, molecular ions, and fragment ions in MS/MS. Favonoids quantitative analyzed by external and internal standard methods through multiple reactions monitoring （MRM） to monitor specific fragment ions and standard curves of three standard substances. The main components in the flavonoids and their contents were apigenin-7-O-β-D-glucuronide （6.66 μg/mg）, hyperoside （2.39 μg/mg）, astragalin （2.30 μg/mg）, scutellarin （1.95 μg/mg）, luteoloside （0.44 μg/mg）, potengriffioside A （0.39 μg/mg）, and isovitexin （0.01 μg/mg）.
出处
《现代食品科技》
EI
CAS
北大核心
2013年第12期3031-3037,共7页
Modern Food Science and Technology
基金
天津市自然科学基金重点项目(120029)
天津市高校科技发展基金项目(20110608)
关键词
西南委陵菜
黄酮
纯化
成分分析
HPLC-ESI-MS
MS
Potentilla fulgens
flavonoids
purification
identification
high performance liquid chromatography-electrospray tandem mass spectrometry
