离子液体-超声辅助萃取／高效液相色谱法测定白花杜鹃叶中的黄酮  

Simultaneous Determination of Flavonoids in Rhododendron Mucronatum Leaves by Ionic Liquid-based Ultrasonic-assisted Extraction Combined with High Performance Liquid Chromatography

作　　者：陈君[1] 周光明[1] 杨远高[1] 秦红英[1] 窦文虎[1] 

机构地区：[1]西南大学化学化工学院,发光与实时分析教育部重点实验室,重庆400715

出　　处：《分析测试学报》2013年第3期341-345,共5页Journal of Instrumental Analysis

基　　金：国家科技重大专项资助(2008ZX07315)

摘　　要：建立了以离子液体1-丁基-3-甲基咪唑溴化盐([BMIM]Br)水溶液为萃取剂,超声辅助萃取结合反相高效液相色谱/紫外检测器同时分离测定白花杜鹃叶中的芦丁、槲皮素和山奈酚3种黄酮化合物的方法。采用Phenomenex C18色谱柱(250 mm×4.6 mm,5μm)进行分离,以乙腈-0.25%乙酸水溶液梯度洗脱,流速1.0 mL.min-1,紫外检测波长355 nm,柱温34℃。在优化条件下,芦丁、槲皮素和山奈酚分别在0.064～128、0.076～152、0.064～128 mg.L-1范围内线性关系良好,相关系数(r)均为0.999 9,检出限(S/N=3)分别为0.006 6、0.009 2、0.005 0 mg.L-1;样品的回收率为90%～97%。实验结果表明,该萃取方法操作简单快速,定量结果准确可靠,且绿色环保,为白花杜鹃叶中黄酮的提取、分离及检测提供了有效的方法。A novel ionic liquid-based ultrasonic-assisted extraction （ILUAE）combined with reversephase high performance liquid chromatography tandem UV detection （ HPLC - UV） was first developed to isolate and determinate flavonoids in rhododendron mucronatum leaves. The 1-butyl-3-methylimid- azolium chloride（ [BMIM] Br） aqueous solution was selected as extraction solvent. The sample was separated on a Phenomenex C_18 column using acetonitrile -0. 25% acetic acid as mobile phase by gradient elution at a flow rate of 1.0 mL·min^-1 The UV detection wavelength was set at 355 nm. The quantitative analysis of rutin, quercetin and kaempferol were carried out by the external standard method. Under the optimal extraction conditions, the calibration curves of rutin, quercetin, and kaempferol were linear in the ranges of 0. 064 - 128, 0. 076 - 152 and 0. 064 - 128 mg· L^--1, re-spectively, with correlation coefficients of 0. 999 9. Their limits of detection （ LODs, S/N = 3 ） were 0. 006 6, 0. 009 2 and 0. 005 0 mg·L^-1, respectively. The spiked recoveries of three compounds ranged from 90% to 97% . The results indicated that the proposed method was an environment-friendly, easy to operation and efficient technique for sample preparation, thus it could provide an alterna- tive means for assaying fiavonoids in the rhododendron mucronatum leaves.

关 键 词：离子液体 超声辅助 高效液相色谱 黄酮 白花杜鹃 

分 类 号：O657.72[理学—分析化学] TQ460.72[理学—化学]