食品科学 ›› 2009, Vol. 30 ›› Issue (14): 171-174.doi: 10.7506/spkx1002-6630-200914032

• 分析检测 • 上一篇    下一篇

固相萃取—离子对液相色谱法测定保健品中的叶酸

吕运开,边 超,王燕桓,秦新英   

  1. 河北大学化学与环境科学学院,河北省分析科学技术重点实验室
  • 收稿日期:2008-10-20 修回日期:2009-01-10 出版日期:2009-07-15 发布日期:2010-12-29
  • 通讯作者: 吕运开 E-mail:lvyunkai@hbu.edu.cn
  • 基金资助:

    国家自然科学基金项目(20675024);第三十七批中国博士后科学基金项目(2005037629);
    河北省教育厅科学计划项目(2006407)

Solid-phase Extraction and Ion-pair RP-HPLC Determination of Folic Acid in Health Food Products

LU Yun-kai,BIAN Chao,WANG Yan-huan,QIN Xin-ying   

  1. Key Laboratory of Analytical Science and Technology of Hebei Province, College of Chemistry and Environmental Science,
    Hebei University, Baoding 071002, China
  • Received:2008-10-20 Revised:2009-01-10 Online:2009-07-15 Published:2010-12-29
  • Contact: LU Yun-kai, E-mail:lvyunkai@hbu.edu.cn

摘要:

建立了一种快速、准确、灵敏的固相萃取- 离子对反相高效液相色谱测定保健品中叶酸的方法。用Chromabond-SB 萃取小柱富集保健品中的叶酸,以四丁基溴化铵为离子对试剂,优化了色谱条件。采用 Lu-Na C18色谱柱(250mm × 4.6mm,5μm),SPD-6AV 紫外可见吸收检测器,流动相为0.05mol/L KH2PO4-0.01mol/L 四丁基溴化铵- 乙腈(88:2:10,V/V),用磷酸调节 pH5.5,流速 1.0ml/min,检测波长284nm。结果表明:叶酸在0.06~2.40μg/ml 浓度范围内,峰面积和浓度呈良好的线性关系,相关系数为0.9996,最小检出限为0.008μg/ml,加标回收率为 95.14%~102.87%。

关键词: 固相萃取, HPLC, 保健品, 叶酸

Abstract:

A simple, rapid, accurate and sensitive method of solid-phase extraction and ion-pair RP-HPLC was developed for the determination of folic acid (FA) in health food products. Solid-phase extraction (SPE) was performed to enrich FA extracted using a Chromabond-SB cartridge with strong anion exchange material. The addition of tetra-n-butylammonium, as an ion-pairing reagent, from samples was found to significantly increase the retention time of FA, thus leading to a well shaped and clearly separated single peak. The analysis was performed on a Lu-Na C18 column (5 μm, 250 mm×4.6 mm) using a mobile phase composed of 0.05 mol/L KH2PO4 solution, 0.01mol/L tetra-n-butylammonium and acetonitrile (88:2:10, V/V, pH 5.5) at a flow rate of 1 ml/min, with the UV detection set at 284 nm. In the range of 0.06-2.40 μg/ml, a good linear relationship between peak area and FA concentration was found, and the correlation coefficient and the LOD were 0.9996 and 0.008 μg/ml, respectively. The spike recoveries for FA in three commercial health food products ranged from 95.14% to 102.87%.

Key words: solid-phase extraction, HPLC, health food products, folic acid

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