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柱前衍生化HPLC测定石榴籽油中石榴酸的含量
Determination of Punicic Acid in Pomegranate Seed Oil by Precolumn Derivatization HPLC
【摘要】 目的:石榴酸(C18∶3)在结构上为顺9,反11,顺13-十八碳三烯酸,为长链烃类,在200~400 nm没有吸收,无法直接用紫外检测器进行检测,本实验采用柱前衍生化方法,使石榴酸带上一个强发色团,使其在200~400 nm有最大吸收,建立石榴籽油中指标性成分石榴酸的柱前衍生化HPLC分析方法。方法:以ω-溴代苯乙酮作为衍生化试剂,以三乙醇胺为相转移催化剂,对石榴籽油进行柱前衍生化,色谱条件采用Diamonsi C18色谱柱(4.6 mm×250 mm,5μm),检测波长272 nm,以甲醇-乙腈-水(68.5∶20∶11.5)为流动相,柱温30℃,流速1.0 m L·min-1。结果:石榴酸在0.026 6~0.133 0 g·L-1(r=0.999)线性关系良好,平均加样回收率为98.7%,RSD 1.8%。结论:该法稳定性、重复性好,定量准确,可作为石榴籽油中石榴酸的定量方法,用于评价和控制石榴籽油的质量。
【Abstract】 Objective: As the long chain hydrocarbons,punicic acid( C18∶ 3) on the structure of 9( Z),11( E),13( Z)-octadecatrienoic acid,which was in 200-400 nm absorption-free and can’t be measured directly by UV detector. This experiment adopted column derivatization methods,made the punicic acid with a strong chromophore in maximum absorption in 200-400 nm. The determination method of punicicacid in pomegranate seed oil by HPLC was established in this thesis. Method: The punicic acid were derivatized with ω-bromoacetophenone as derivative reagent,triethanolamine as catalyst,the Diamonsi C18column( 4. 6 mm × 250 mm,5 μm) was used. The detection wavelength was set at 272 nm,column temperature 30 ℃,with methanolacetonitrile-water( 68. 5∶ 20∶ 11. 5) aseluent,the flow rate was 1. 0 m L·min- 1. Result: The standard curves of punicic acid is linear within in the range of 0. 026 6-0. 133 0 g·L- 1and the coefficient is 0. 999. The average recovery of punicic acid is 98. 7%,RSD is 1. 8%. Conclusion: The method is reproducible and accurate,which can be used as the determination method of punicic acid inpomegranate seed oil,and used for the quality control of pomegranate seed oil.
【Key words】 pomegranate seed oil; punicic acid; precolumn derivatization; HPLC;
- 【文献出处】 中国实验方剂学杂志 ,Chinese Journal of Experimental Traditional Medical Formulae , 编辑部邮箱 ,2015年04期
- 【分类号】R284.1;O657.72
- 【被引频次】1
- 【下载频次】155