食品科学 ›› 2016, Vol. 37 ›› Issue (20): 37-41.doi: 10.7506/spkx1002-6630-201620007

• 成分分析 • 上一篇    下一篇

离子液体辅助超声萃取-高效液相色谱同时测定半边莲中6 种黄酮类化合物

邓永利,周光明,陈军华,高 意,廖安辉   

  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
  • 收稿日期:2016-10-27 修回日期:2016-10-27 出版日期:2016-10-25 发布日期:2016-12-01
  • 通讯作者: 周光明
  • 基金资助:

    中央高校基本科研业务费专项(100030-2120130993)

Simultaneous Determination of 6 Flavonoid Compounds in Herba Lobelia chinensis by High Performance Liquid Chromatography after Ionic Liquid Assisted Ultrasonic Extraction

DENG Yongli, ZHOU Guangming, CHEN Junhua, GAO Yi, LIAO Anhui   

  1. Key Laboratory on Luminescence and Real-Time Analysis, Ministry of Education,
    School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715, China
  • Received:2016-10-27 Revised:2016-10-27 Online:2016-10-25 Published:2016-12-01
  • Contact: ZHOU Guangming

摘要:

目的:通过单因素试验和正交试验对离子液体辅助萃取半边莲中黄酮类化合物的条件进行优化,建立高效液相色谱法同时分离测定半边莲中芦丁、槲皮素、柚皮素、橙皮素、山柰酚和芹菜素的方法。方法:采用InertSustain C18色谱柱(150 mm×4.6 mm,5 μm)进行分离;流动相为甲醇(B)-乙酸溶液(A,pH 3.0),梯度洗脱;流速1.0 mL/min;紫外检测波长285 nm;柱温35 ℃。结果:以黄酮类化合物的提取量为指标,最佳提取条件为甲醇体积分数80%、固液比1∶80(g/mL)、萃取时间30 min、离子液体浓度0.6 mol/L。在优化的色谱条件下,芦丁、槲皮素、柚皮素、橙皮素、山柰酚和芹菜素分离效果良好;定性检出限(RSN = 3)依次为0.001 2、0.002 3、0.002 6、0.000 2、0.001 0、0.000 6 μg/mL;样品回收率为91.77%~102.53%。结论:该萃取方法操作简单快速,为半边莲中黄酮类化合物的提取分离及检测提供了有效的方法。

关键词: 高效液相色谱, 半边莲, 黄酮类化合物, 离子液体, 超声萃取

Abstract:

Objectives: To optimize the conditions for ionic liquid-assisted extraction of flavonoids compounds from Herba
Lobelia chinensis using single factor and orthogonal array designs and consequently to establish a high performance liquid
chromatography (HPLC) method for simultaneous determination of rutin, quercetin, naringgenin, hesperetin, kaempferol and
apigenin in Herba Lobelia chinensis. Methods: The 6 compounds were separated on an InertSustain C18 (150 mm × 4.6 mm, 5 μm)
using a mobile phase consisting of methanol and acetic acid (pH 3.0) with gradient elution at a flow rate of 1.0 mL/min.
The detection wavelength was set at 285 nm. The column temperature was maintained at 35 ℃. Results: The optimum
extraction conditions for total flavonoids were determined as follows: 80% (V/V) aqueous methanol as extraction solvent;
solid-to-liquid ratio, 1:80 (g/mL); extraction time, 30 min; and ionic liquid concentration, 0.6 mol//L. Under these conditions,
rutin, quercetin, naringgenin, hesperetin, kaempferol and apigenin were separated satisfactorily. The limits of detection (LODs)
for these flavonoid compounds were 0.001 2, 0.002 3, 0.002 6, 0.000 2, 0.001 0 and 0.000 6 μg/mL, respectively. The recoveries
of spiked samples ranged from 91.77% to 102.53%. Conclusion: The proposed method is simple and rapid, and it can provide an
efficient means for the extraction, separation and determination of flavonoid compounds in Herba Lobelia chinensis.

Key words: high performance liquid chromatography, Herba Lobelia chinensis Lour., flavonoid compounds, ionic liquid, ultrasonic extraction

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