食品科学 ›› 2012, Vol. 33 ›› Issue (24): 215-218.doi: 10.7506/spkx1002-6630-201224044

• 分析检测 • 上一篇    下一篇

离子液体-超声辅助萃取-高效液相色谱测定桑叶中的黄酮

陈君,周光明*,杨远高,张丽贤   

  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:2011-10-23 修回日期:2012-11-14 出版日期:2012-12-25 发布日期:2012-12-12
  • 通讯作者: 陈君 E-mail:chenjun9@swu.edu.cn
  • 基金资助:

    国家科技重大专项

Ionic Liquid-based Ultrasonic-Assisted Extraction Coupled with HPLC for Sensitive Determination of Flavonoids in Mulberry Leaves

CHEN Jun,ZHOU Guang-ming*,YANG Yuan-gao,ZHANG Li-xian   

  1. Key Laboratory on Luminescence and Real-Time Analysis, Ministry of Education, College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715, China
  • Received:2011-10-23 Revised:2012-11-14 Online:2012-12-25 Published:2012-12-12
  • Contact: Jun CHEN E-mail:chenjun9@swu.edu.cn

摘要: 目的:建立以离子液体1-丁基-3-甲基咪唑溴化盐([BMIM]Br)为萃取剂,结合超声辅助萃取,利用高效液相色谱法同时分离测定桑叶中的桑色素、槲皮素和山奈酚3种黄酮的方法。方法:采用Phenomenex C18色谱柱(250mm×4.6mm,5μm);流动相为甲醇-0.1%磷酸溶液,采用梯度洗脱;流速1.0mL/min;紫外检测波长365nm;柱温为34℃。结果:该方法对桑色素、槲皮素和山奈酚分别在0.0065~130、0.0064~128、0.0042~84μg/mL范围内线性关系良好,相关系数(r)均大于0.9998,检出限(RSN=3)依次为0.99、1.31、0.64ng/mL;样品回收率为90.00%~95.31%。结论:本法操作简单快速、定量准确、灵敏度高、成本低、且对环境友好,为桑叶中黄酮化合物的检测及分离提供了一个有效的科学方法。

关键词: 离子液体, 超声辅助, 高效液相色谱, 黄酮, 桑叶

Abstract: An analytical method to determine flavonoids such as morin hydrate, quercetin and kaempferol in mulberry leaves was proposed using ultrasonic-assisted extraction coupled with HPLC. The extraction solvent used was 1-butyl-3-methylimidazolium chloride ([BMIM]Br). The chromatographic separation was performed on Phenomenex C18 column (250 mm × 4.6 mm, 5 μm) using a mobile phase made up of methanol and 0.1% phosphoric acid at a flow rate of 1.0 mL/min by gradient elution. The detection wavelength and column temperature were set as 365 nm and 34 ℃, respectively. This method showed good linearity in the range of 0.0065–130 μg/mL (r = 0.9999) for morin hydrate, of 0.0064–128 μg/mL (r = 0.9999) for quercetin, and of 0.0042–84 μg/mL for kaempferol. The limit of detection, LOD, (RSN = 3) of this method was 0.99, 1.31 ng/mL and 0.64 ng/mL for morin hydrate, quercetin and kaempferol, respectively. Average recoveries ranging 90.00% to 95.31% were obtained for these three flavonoids (n = 3). This method was simple, fast, accurate, sensitive, cheap and environment-friendly and could provide a scientific way to determine flavonoids in mulberry leaves.

Key words: ionic liquid, ultrasonic assistance, HPLC, flavonoids, mulberry leaves

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