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化学学报
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化学学报 ›› 2006, Vol. 64 ›› Issue (24): 2461-2466. 上一篇    下一篇

研究论文

高效液相色谱化学发光法检测牛奶中残留四环素类化合物的研究

张琰图1,2, 章竹君*,1, 孙永华1   

  1. (1陕西师范大学化学与材料科学学院 西安 710062)
    (2延安大学化学化工学院 延安 716000)
  • 投稿日期:2006-03-08 修回日期:2006-04-03 发布日期:2006-12-28
  • 通讯作者: 章竹君

Determination of Tetracyclines Residues in Milk Using High Per-formance Liquid Chromatography with Chemiluminescence Detection

ZHANG Yan-Tu1,2; ZHANG Zhu-Jun*,1; SUN Yong-Hua1   

  1. (1 Department of Chemistry, School of Chemistry and Materials Science, Shaanxi Normal University, Xi'an 710062)
    (2 Department of Chemistry and Chemical Engineering, Yan'an University, Yan'an 716000)
  • Received:2006-03-08 Revised:2006-04-03 Published:2006-12-28
  • Contact: ZHANG Zhu-Jun

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被引次数

114

基于四环素类抗生素药物中的四环素(TC)、土霉素(OTC)、金霉素(CTC)和多西环素(DC)能够强烈增敏通过恒电流电解方法在线电生BrO－和鲁米诺之间产生的化学发光, 提出了一种高效液相色谱(HPLC)化学发光(CL)法检测4种四环素类抗生素药物的新方法. 以Nucleosil RP-C18 (250 mm×4.6 mm, i.d., 5 μm, pore size, 100 Å)为色谱柱, 0.05 mol• L－1磷酸二氢钾(pH 2.5)-乙腈(30∶70, V∶V)为流动相, 流速1.2 mL/min, 柱温25 ℃, 同时分离检测四种抗生素的总时间为11 min. 研究并优化了流动相、电生试剂化学发光检测的条件. 四种抗生素的检出限为0.002～0.008 μg•mL－1 (3σ), 对0.01 μg•mL－1的四种抗生素测定的相对标准偏差为2.0%～3.6% (n＝11). 该方法已成功应用于牛奶中残留四环素类抗生素含量的分析.

关键词: 四环素类抗生素, 化学发光检测器, 在线电生BrO－, 高效液相色谱, 牛奶

A novel method for the determination of four tetracycline antibiotics (TCs) including tetracycline (TC), oxytetracycline (OTC), chlortetracycline (CTC) and doxycycline (DC) by means of high-performance liquid chromatography (HPLC) with chemiluminescence (CL) detection was proposed. The method was based on the enhancement effect of TCs on the chemiluminescence reaction between luminol and BrO－, which was on-line electrogenerated by constant current electrolysis. The separation was carried out on Nucleosil RP-C18 column (250 mm×4.6 mm i.d., 5 μm, pore size, 100 Å) at 25 ℃. The mobile phase consisted of a V(acetonitrile)∶V(0.05 mol•L－1 potassium dihydrogen phosphate buffer, pH 2.5)＝30∶70 solution. At a flow-rate of 1.2 mL/min, the total run time was 11 min. The effects of several parameters on the HPLC resolution and CL emission were studied systematically. For the four TCs, the detection limits at a signal-to-noise of 3 ranged from 0.002 to 0.008 μg•mL－1. The relative standard deviations for the determination of TCs ranged from 2.0% to 3.6% (n＝11, c＝0.01 μg•mL－1). The method has been satis-factorily applied to the analysis of spiked raw milk samples.

Key words: tetracycline antibiotic, chemiluminescence detector, on-line electrogenerated BrO－, high per-formance liquid chromatography, milk