色谱

色谱 ›› 2010, Vol. 28 ›› Issue (10): 945-949.DOI: 10.3724/SP.J.1123.2010.00945

• 研究论文 • 上一篇    下一篇

固相萃取-高效液相色谱法测定蜂蜜中的有机酸

朱晓玲1,2, 叶飞1,2, 杨洁1,2, 肖潇4, 文红2,3*, 刘睿1,2*   

  1. 1. 华中农业大学食品科技学院, 湖北 武汉 430070; 2. 武汉市蜂产品质量控制工程技术研究中心, 湖北 武汉 430070; 3. 湖北省产品质量监督检验研究院, 湖北 武汉 430061; 4. 湖南农业大学食品科技学院, 湖南 长沙 410128
  • 收稿日期:2010-07-01 修回日期:2010-08-20 出版日期:2010-10-28 发布日期:2010-10-28
  • 通讯作者: 文红,硕士,高级工程师,研究方向为食品质量分析. E-mail: wen_red@sina.com.刘 睿,博士,副教授,研究方向为蜂产品加工及蜂产品质量控制. E-mail: liurui@mail.hzau.edu.cn.
  • 基金资助:

    武汉市科技局工程技术研究中心项目(No. 200920137007)和华中农业大学新兴学科研究生教育发展基金(No. 200922).

Determination of organic acids in honey by solid phase extraction-high performance liquid chromatography

ZHU Xiaoling1,2, YE Fei1,2, YANG Jie1,2, XIAO Xiao4, WEN Hong2,3*, LIU Rui1,2*   

  1. 1. College of Food Science and Technology, Huazhong Agricultural University, Wuhan 430070, China; 2. Wuhan Research Center on Quality Control Engineering of Bee Products, Wuhan 430070, China; 3. Hubei Provincial Supervision and Inspection Research Institute for Product Quality, Wuhan 430061, China; 4. College of Food Science and Technology, Hunan Agricultural University, Changsha 410128, China
  • Received:2010-07-01 Revised:2010-08-20 Online:2010-10-28 Published:2010-10-28

PDF

1032

被引次数

34

摘要： 建立了固相萃取-高效液相色谱(SPE-HPLC)同时测定蜂蜜中5种有机酸(L-苹果酸、马来酸、琥珀酸、柠檬酸、D-苹果酸)含量的方法。蜂蜜经制样后过Bond Elutes SAX固相萃取(SPE)小柱净化,用C18-MS-II反相色谱柱(250 mm×4.6 mm, 5 μm)进行分离,流动相为2%偏磷酸溶液,流速为0.7 mL/min,检测波长为210 nm。在此条件下5种有机酸在相应的线性范围内其线性相关系数均大于0.9967;方法的回收率为86.0%～103.9%,相对标准偏差为5.7%～9.8%(n=6),检出限为0.06～9.4 mg/kg。所建立的方法可用于蜂蜜样品中有机酸的测定。

关键词: 反相高效液相色谱法, 蜂蜜, 固相萃取, 有机酸

Abstract: A method for the simultaneous determination of 5 organic acids (L-malic acid, maleic acid, succinic acid, citric acid, D-malic acid) in honey was developed by solid-phase extraction and high performance liquid chromatography (SPE-HPLC). The sample was purified by a Bond Elutes SAX SPE cartridge after pretreatment, then separated using a reversed-phase C18-MS-IIcolumn. A 2% metaphosphoric acid solution was used as the mobile phase at a flow rate of 0.7 mL/min. The detection was performed by a diode array detector at 210 nm. Under these conditions, the linear ranges of the method for L-malic acid was 5.0~500 mg/L, for maleic acid was 0.1~500 mg/L, and for succinic acid, citric acid, D-malic acid were 18.0~500 mg/L. The correlation coefficients of 5 organic acids were more than 0.9967. The average recoveries of 5 organic acids were 86.0%~103.9% with the relative standard deviations of 5.7%~9.8% (n=6). The detection limits ranged from 0.06 to 9.4 mg/kg. The method can be used for determining organic acids in honey samples.

Key words: honey, organic acids, reversed-phase high performance liquid chromatography (RP-HPLC), solid-phase extraction (SPE)