食品科学 ›› 2009, Vol. 30 ›› Issue (16 ): 258-261.doi: 10.7506/spkx1002-6630-200916057

• 分析检测 • 上一篇    下一篇

反相高效液相色谱法检测不同品种和叶位桑叶中1- 脱氧野尻霉素

魏兆军,蒋 磊,周乐春,汪爱民,张 松   

  1. 合肥工业大学生物与食品工程学院
  • 收稿日期:2009-04-26 出版日期:2009-08-15 发布日期:2010-12-29
  • 通讯作者: 魏兆军, E-mail:zjwei@hfut.edu.cn
  • 基金资助:

    安徽省教育厅省级重大自然科学基金项目(ZD2008007-2);教育部新世纪优秀人才基金项目(NCET-07-0251);安徽省第四批优秀青年科技基金项目(08040106803)

RP-HPLC Detection of 1-Deoxynojirimycin in Different Varieties and Sites of Mulberry Leaves

WEI Zhao-jun,JIANG Lei,ZHOU Le-chun,WANG Ai-min,ZHANG Song   

  1. School of Biotechnology and Food Engineering, Hefei University of Technology, Hefei 230009, China
  • Received:2009-04-26 Online:2009-08-15 Published:2010-12-29
  • Contact: WEI Zhao-jun, E-mail:zjwei@hfut.edu.cn
  • Supported by:

    安徽省教育厅省级重大自然科学基金项目(ZD2008007-2);教育部新世纪优秀人才基金项目(NCET-07-0251);
    安徽省第四批优秀青年科技基金项目(08040106803)

摘要:

建立以芴甲氧酰氯(FMOC-Cl)为衍化剂的柱前衍生化- 反相高效液相紫外线检测法测定桑叶中1- 脱氧野尻霉素(DNJ)含量的方法,并对不同品种、不同叶位桑叶中DNJ 含量进行检测。结果表明:以0.05mol/L HCl 为溶剂提取桑叶粉中的DNJ,用芴甲氧酰氯(FMOC-Cl)为衍生化试剂,在pH8.50 硼酸盐缓冲液条件下,衍生化和RPHPLC检测效果最好。反相高效液相色谱- 紫外检测法检测DNJ 时,流动相中乙腈:0.1%醋酸为55:45(V/V)时色谱分离效果最好,DNJ-FMOC 的峰面积与DNJ 浓度呈高度正相关关系,相关系数为0.9852。不同品种的桑叶中DNJ含量不同,本研究的15 个样品中青阳青桑的DNJ 含量最高,达到0.1486%,皮桑含量最低,为0.04291%。不同叶位桑叶的DNJ 含量不同,第1 叶位至第5 叶位桑叶的DNJ 含量逐渐降低,说明桑叶随着发育成熟,DNJ 的含量逐渐降低。结果显示该方法快捷、稳定、灵敏、准确度高,适合桑叶中DNJ 含量的检测。

关键词: 桑叶, 1- 脱氧野尻霉素, 反相高效液相色谱, 衍生化

Abstract:

A method of pre-column derivatization with FMOC-Cl followed by RP-HPLC with UV detection was established for the determination of 1-deoxynojirimycin (DNJ) content in different varieties and sites of mulberry leaves. DNJ was extracted from mulberry leaves using 0.05 mol/L HCl and derivatized using FMOC-Cl in borate buffer solution (pH 8.50) prior to RP-HPLC detection. The chromatographic separation was achieved on a Waters X-Terra column using a mobile phase consisting of a mixture of acetonitrile and 0.1% aqueous acetic acid (55:45, V/V). There was a high positive correlation between the peak area and concentration of DNJ-FMOC with a correlation coefficient of 0.9852. The DNJ content was varied in different varieties of mulberry leaves. Among 15 varieties of mulberry, Qingyang Qing mulberry leaves contained the highest DNJ (0.1486%), while Pi mulberry leaves the lowest (0.04291%). Also, mulberry leaves in different sites contained different DNJ contents. It decreased from the top to bottom gradually, indicating DNJ content is reduced with the maturation of mulberry leaves.

Key words: mulberry leaves, 1-deoxynojirimycin (DNJ), RP-HPLC, derivatization

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