色谱

色谱 ›› 2012, Vol. 30 ›› Issue (08): 792-797.DOI: 10.3724/SP.J.1123.2012.03048

• 研究论文 • 上一篇    下一篇

柱后衍生-高效液相色谱法测定玉米中伏马菌素B1和B2

张晓旭1, 肖志勇2, 张红艳3,4, 杨丽丽1, 马丽艳1,4*   

  1. 1. 中国农业大学食品科学与营养工程学院, 北京 100083; 2. 北京市农业环境监测站, 北京 100029; 3. 中国农业大学理学院, 北京 100193; 4. 农业部农产品质量监督检验测试中心, 北京 100083
  • 收稿日期:2012-03-25 修回日期:2012-05-07 出版日期:2012-08-28 发布日期:2012-08-17
  • 通讯作者: 马丽艳,高级实验师,主要从事食品安全及其检测工作. Tel: (010)62737375, E-mai: lyma1203@cau.edu.cn.
  • 基金资助:

    农业行业标准制定项目.

Determination of fumonisins B1 and B2 in corn by high performance liquid chromatography with post-column derivatization method

ZHANG Xiaoxu1, XIAO Zhiyong2, ZHANG Hongyan3,4, YANG Lili1, MA Liyan1,4*   

  1. 1. College of Food Science and Nutritional Engineering, China Agricultural University, Beijing 100083, China; 2. Beijing Agro-Environmental Monitoring Station, Beijing 100029, China; 3. College of Science, China Agricultural University, Beijing 100193, China; 4. Supervision & Testing Center for Agricultural Products Quality, Ministry of Agriculture, Beijing 100083, China
  • Received:2012-03-25 Revised:2012-05-07 Online:2012-08-28 Published:2012-08-17

PDF

450

被引次数

9

摘要： 建立了邻苯二甲醛(OPA)柱后衍生-高效液相色谱测定玉米中伏马菌素B1和B2(FB1和FB2)的方法。采用ZORBAX SB-C18色谱柱,以0.1 mol/L磷酸二氢钠溶液(pH 3.3)-甲醇为流动相,梯度洗脱。流动相流速为0.8 mL/min,柱温40 ℃;衍生剂的流速为0.4 mL/min,衍生温度为室温。实验对衍生剂缓冲液的pH、衍生剂的浓度和流速、激发和发射波长等重要条件进行了优化。结果表明,衍生剂的pH在10.5、OPA的质量浓度为2 g/L、流速为0.4 mL/min、激发波长335 nm、发射波长440 nm时测定效果良好,FB1、FB2在0.2～20 mg/L范围内线性关系良好,相关系数大于0.999; FB1和FB2的检出限均为0.02 mg/kg;在0.1～ 4.0 mg/kg范围内,3个添加水平的平均回收率为82.5%～89.8%。该方法精确、简单、快速,适合玉米中FB1和FB2的测定。

关键词: 伏马菌素, 高效液相色谱, 邻苯二甲醛, 玉米, 柱后衍生

Abstract: A high performance liquid chromatography-fluorescence detection with post-column derivatization method was developed to detect fumonisin B1 (FB1) and fumonisin B2 (FB2) in corn. Several factors, such as the pH of derivatization buffer, concentration and flow rate of derivatization reagents, excitation wavelength, emission wavelength, which affected the detection of fumonisins were optimized. The separation was performed on a ZORBAX SB C18 column operated at 40 ℃ with the gradient elution by two mobile phases of 0.1 mol/L sodium dihydrogen phosphate solution (pH 3.3) and methanol at a flow rate of 0.8 mL/min. The derivatization was performed at ambient temperature. The o-phthalaldehyde (OPA) flow rate was 0.4 mL/min. The results showed that the optimum conditions were pH 10.5 of the derivatization reagent, OPA concentration at 2 g/L, and excitation wavelength of 335 nm, emission wavelength of 440 nm. The linear plots of FB1 and FB2 were obtained between 0.2 to 20 mg/L, with the correlation coefficients above 0.999 for both FB1 and FB2. The limits of detection of fumonisins B1 and B2 were 0.02 mg/kg. The mean recoveries at the three spiked levels of 0.1~4.0 mg/kg were 82.5%~89.8%. This method is accurate, simple, rapid and suitable for the determination of fumonisins B1 and B2 in corn.

Key words: corn, fumonisins, o-phthalaldehyde (OPA), post-column derivatization, high performance liquid chromatography (HPLC)

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