Liquid chromatography on an amide stationary phase with post-column derivatization and fluorimetric detection for the determination of streptomycin and dihydrostreptomycin in foods.
Liquid chromatography on an amide stationary phase with post-column derivatization and fluorimetric detection for the determination of streptomycin and dihydrostreptomycin in foods.
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DOI：
10.1016/j.talanta.2006.12.006
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发表时间：
2007-04
期刊：
影响因子：
6.1
通讯作者：
P. Viñas;N. Balsalobre;M. Hernández-Córdoba
中科院分区：
文献类型：
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作者：
P. Viñas;N. Balsalobre;M. Hernández-Córdoba
本文提出用离子对液相色谱法分离链霉素及其衍生物双氢链霉素。该方法是基于使用一种新的固定相的基础上的配体与酰胺基团和封端的三甲基硅烷基，避免出现拖尾峰。等度移动的流动相由6：94（v/v）乙腈/10 mM戊磺酸（pH 3.3）混合物组成，流速为1 mL min − 1，荧光检测涉及使用β-萘醌-4-磺酸盐的柱后衍生反应。线性、精密度、回收率和灵敏度均符合要求。该方法已应用于蜂蜜、牛奶、鸡蛋、肝脏等食品中氨基糖苷类抗生素的分析。通过酸水解进行提取以释放蛋白质结合的抗生素。链霉素和双氢链霉素在食物样本中的检出限分别为7.5和15微克/千克。
The separation of streptomycin and its derivative dihydrostreptomycin using ion-pair liquid chromatography is proposed. The method is based on the use of a new stationary phase based on a ligand with amide groups and the endcapping of trimethylsilyl which avoids the appearance of tailed peaks. The isocratic mobile phase consisted of a 6:94 (v/v) acetonitrile/10mM pentanesulfonic acid (pH 3.3) mixture at a flow-rate of 1mLmin−1and fluorescence detection involved a post-column derivatization reaction using β-naphthoquinone-4-sulfonate. Linearity, precision, recovery and sensitivity were satisfactory. The procedure was applied to the analysis of the aminoglycoside antibiotics in different types of foods, as honey, milk, egg and liver. Extraction was carried out by acidic hydrolysis to release protein-bound antibiotics. Detection limits in the food samples are 7.5 and 15μgkg−1for streptomycin and dihydrostreptomycin, respectively.