辣椒中β-隐黄质的分离制备  

Preparation of β-Cryptoxanthin from Paprika

作　　者：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] 

机构地区：[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

出　　处：《食品科学》2013年第6期10-13,共4页Food Science

基　　金：国家自然科学基金项目(31040063);山东省科技攻关项目(2010GSF10287);济南高等院所自主创新计划项目(201004010)

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。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 fl-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.

关 键 词：辣椒 β-隐黄质 制备高效液相色谱 

分 类 号：TS255.1[轻工技术与工程—农产品加工及贮藏工程]