Determination of Doxycycline, 4-epidoxycycline, and 6-epidoxycycline in Aquatic Animal Muscle Tissue by an Optimized Extraction Protocol and Ultra-performance Performance Liquid Chromatography with Ultraviolet Detection

文献类型： 外文期刊

第一作者： Xu, Ning

作者： Xu, Ning;Dong, Jing;Zhou, Wei;Liu, Yongtao;Ai, Xiaohui;Xu, Ning;Dong, Jing;Zhou, Wei;Liu, Yongtao;Ai, Xiaohui;Xu, Ning;Dong, Jing;Zhou, Wei;Liu, Yongtao;Ai, Xiaohui;Ai, Xiaohui

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关键词： Aquatic animal muscle; doxycycline; QuEChERS; ultra-performance liquid chromatography

期刊名称：ANALYTICAL LETTERS （ 影响因子：2.329； 五年影响因子：1.738 ）

ISSN： 0003-2719

年卷期： 2019 年 52 卷 3 期

页码：

收录情况： SCI

摘要： A fast ultra-performance liquid chromatography method was developed for the separation and quantification of doxycycline, 4-epidoxycycline, and 6-epidoxycycline in the muscles of channel catfish, shrimp, eel and turtle. The analytes were separated by comprehensive optimization of the chromatographic conditions. The extraction method was performed using a modified QuEChERS methodology. 2 g of muscle sample were mixed with 5 mL Mcllvaine buffer (pH 4), and 4 g of sodium sulfate and 2 g of sodium chloride were added for liquid-liquid partitioning. The mixture was agitated for 30 s and extracted with 10 mL of acidified acetonitrile. The resulting extract was purified using 200 mg of a C-18-silica adsorbent. The samples were analyzed using ultra-performance liquid chromatography with ultraviolet detection using a BEH C18 column (2.1 mm x100 mm, 1.7 mu m). The limits of detection were less than 25 mu g/kg and the limits of quantitation were less than 50 mu g/kg for all analytes. The recoveries of the analytes were from 62.3% to 89.0% with relative standard derivations below 10.0%. The method provided efficient extraction and purification that enabled rugged and low-cost determination of the analytes.

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