Fluorometric Determination of Tetracyclines in Honey by High Performance Liquid Chromatography
Fluorometric Determination of Tetracyclines in Honey by High Performance Liquid Chromatography
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高效液相色谱荧光法测定蜂蜜中的四环素类药物
DOI：
10.3358/shokueishi.32.43
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发表时间：
1991
期刊：
影响因子：
--
通讯作者：
N. Tanahashi
中科院分区：
文献类型：
--
作者：
K. Nakaya;Yoshio Kobayashi;N. Tanahashi
建立了高效液相色谱荧光检测器测定蜂蜜中土霉素（OTC）和金霉素（CTC）的灵敏、选择性方法。将蜂蜜样品溶解在0.1N盐酸中，通过Sep-Pak C18小柱。用水洗涤柱后，用甲醇洗脱OTC和CTC并通过反离子萃取纯化。将分离的OTC用醋酸镁-巴比妥钠溶液处理，CTC用0.05M KOH处理，得到荧光衍生物。 OTC 和 CTC 在 Asahipak Gel ODP-50 柱上分离，并通过荧光测定法定量。 OTC 的流动相为含有 20mM 1-庚烷磺酸钠（最终浓度）的 0.1M 甘氨酸缓冲液 (pH 10)-甲醇 (20:1)，CTC 的流动相为 0.01M 甘氨酸缓冲液 (pH 10)-甲醇 (5:1)。以 0.5ppm 和 1ppm 的水平添加到蜂蜜中的 OTC 和 CTC 的回收率为 68.5， OTC 为 73.2%，CTC 分别为 53.1 和 68.1%。 OTC 的检测限为 0.02ppm，CTC 的检测限为 0.005ppm。
A sensitive and selective method for determination of oxytetracycline (OTC) and chlortetracycline (CTC) in honey by high performance liquid chromatography with a fluorescence detector was developed.A honey sample was dissolved in 0.1N hydrochloric acid and passed through a Sep-Pak C18 cartridge. After washing of the cartridge with water, OTC and CTC were eluted with methanol and purified by counter-ion extraction. The isolated OTC was treated with magnesium acetate-sodium barbital solution and CTC was treated with 0.05M KOH to obtain a fluorescent derivative. OTC and CTC were separated on an Asahipak Gel ODP-50 column and quantitated by fluorometry. The mobile phase for OTC was 0.1M glycine buffer (pH 10)-methanol (20:1) containing 20mM sodium 1-heptane-sulfonate (final concentration) and that for CTC was 0.01M glycine buffer (pH 10)-methanol (5:1).The recoveries of OTC and CTC added to honey at levels of 0.5ppm and 1ppm were 68.5 and 73.2% for OTC, and 53.1 and 68.1% for CTC, respectively. The limits of detection were 0.02ppm for OTC and 0.005ppm for CTC.