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采用高锰酸钾-亚硫酸钠-β-环糊精化学发光检测的高效液相色谱法测定蜂蜜中的四环素残留量

Determination of tetracyclines residues in honey using high-performance liquid chromatography with potassium permanganate-sodium sulfite-beta-cyclodextrin chemiluminescence detection.

作者信息

Wan Guo-Hui, Cui Hua, Zheng Hai-Song, Zhou Jian, Liu Li-Juan, Yu Xiao-Feng

机构信息

Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026, PR China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Sep 25;824(1-2):57-64. doi: 10.1016/j.jchromb.2005.06.039.

Abstract

A novel method was developed for the simultaneous determination of tetracycline antibiotic (TCA) residues such as oxytetracycline (OTC), tetracycline (TC), and metacycline (MTC) by high-performance liquid chromatography (HPLC) coupled with chemiluminescence (CL) detection. The procedure was based on the chemiluminescent enhancement by TCAs of the potassium permanganate-sodium sulfite-beta-cyclodextrin system in a phosphoric acid medium. The separation was carried out with an isocratic elution using a mixture of acetonitrile and 0.001 M phosphoric acid. For the three TCAs, the detection limits at a signal-to-noise of 3 ranged from 0.9 to 5.0 ng/ml. The relative standard deviations for the determination of TCAs ranged from 3.1 to 7.4% within a day (n=11) and ranged from 2.2 to 8.6% in 3 days (n=9), respectively. The method was successfully applied to the determination of TCA residues in honey samples. The possible mechanism of the CL reaction was also discussed.

摘要

开发了一种通过高效液相色谱(HPLC)与化学发光(CL)检测联用同时测定四环素类抗生素(TCA)残留量的新方法,这些残留包括土霉素(OTC)、四环素(TC)和甲烯土霉素(MTC)。该方法基于在磷酸介质中,TCA对高锰酸钾-亚硫酸钠-β-环糊精体系化学发光的增强作用。采用乙腈和0.001M磷酸的混合物进行等度洗脱以实现分离。对于这三种TCA,信噪比为3时的检测限在0.9至5.0 ng/ml之间。一天内(n = 11)测定TCA的相对标准偏差在3.1%至7.4%之间,三天内(n = 9)相对标准偏差在2.2%至8.6%之间。该方法成功应用于蜂蜜样品中TCA残留量的测定。还讨论了CL反应的可能机理。

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