食品科学 ›› 2013, Vol. 34 ›› Issue (6): 10-13.doi: 10.7506/spkx1002-6630-201306003

• 工艺技术 • 上一篇    下一篇

辣椒中β-隐黄质的分离制备

井凤1,2,王丽1,2,徐双双1,2,耿岩玲1,王明林2,王晓1,2,   

  1. 1.山东省科学院分析测试中心,山东 济南 250014;2.山东农业大学食品科学与工程学院,山东 泰安 271018
  • 收稿日期:2011-12-06 修回日期:2013-01-30 出版日期:2013-03-25 发布日期:2013-03-01
  • 通讯作者: 王晓 E-mail:wangx@keylab.net
  • 基金资助:
    辣椒干制过程中红变机制及调控;中药药效物质标准化制备的技术体系研究;中药药效物质标准化制备的技术体系研究

Preparation of β-Cryptoxanthin from Paprika

JING Feng1,2,WANG Li1,2,XU Shuang-shuang1,2,GENG Yan-ling1,WANG Ming-lin2,WANG Xiao1,2,   

  1. 1. Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan 250014, China;2. College of Food Science and Engineering, Shandong Agricultural University, Taian 271018 , China
  • Received:2011-12-06 Revised:2013-01-30 Online:2013-03-25 Published:2013-03-01

摘要: 建立从辣椒中分离制备高纯度β-隐黄质的方法。辣椒粉先经丙酮超声提取、皂化,硅胶柱色谱进行粗分后进一步采用制备液相对β-隐黄质分离制备。通过紫外光、电喷雾电离质谱、核磁共振氢谱和核磁共振碳谱对所分离的β-隐黄质进行结构鉴定,分析型高效液相色谱进行纯度测定。结果表明:每5g辣椒色素浸膏与异丙醇的比例为1:9(g/mL)、加入6.5mL质量浓度为20g/100mL的KOH-甲醇溶液,在室温条件下皂化24h,皂化完全;硅胶柱色谱进行粗分时用石油醚与丙酮作为洗脱溶剂,当体积比为10:1时,β-隐黄质得到较好的富集;制备液相的条件为丙酮-水(95:5,V/V)、流速5mL/min,可制备分离出纯度为99.0%的β-隐黄质单体。该方法简便快捷、重现性好、所得β-隐黄质纯度高,可作为β-隐黄质的分离制备研究。

关键词: 辣椒, β-隐黄质, 制备高效液相色谱

Abstract: In order to establish a method for the separation and preparation of β-cryptoxanthin from paprika, the crude β-cryptoxanthin was extracted by ultrasonic acetone extraction, saponificated and separated by silica gel column chromatography. Preparative high performance liquid chromatography was used to refine and purify β-cryptoxanthin. The structure of β-cryptoxanthin was identified by UV, ESI-MS, 1H-NMR and 13C-NMR. The purity of β-cryptoxanthin was determined by analytical HPLC. The results indicated that complete saponification of chili pigment extract was achieved when saponifying its dispersion in 45 mL of isopropanol (9 g/mL) with 6.5 mL of 20% KOH methanol solution for 24 h at room temperature. During the rough separation by silica gel column chromatography using petroleum ether and acetone as elution solvents, β-cryptoxanthin could be better enriched at a volume ratio of 10:1. The preparative high performance liquid chromatography required acetone and water at a ratio of 95:5 (V/V) and a flow rate of 5 mL/min. Under these optimized conditions, β-cryptoxanthin with a purity of 99.0% could be obtained. This developed method is simple, rapid, reproductive, and suitable for the preparation of β-cryptoxanthin with high purity.

Key words: paprika, β-cryptoxanthin, preparative HPLC

中图分类号: