采用柱前甲醛衍生化液相色谱法测定鲶鱼和鲑鱼组织中的阿莫西林。
Determination of amoxicillin in catfish and salmon tissues by liquid chromatography with precolumn formaldehyde derivatization.
作者信息
Ang C Y, Luo W, Hansen E B, Freeman J P, Thompson H C
机构信息
National Center for Toxicological Research, U.S. Food and Drug Administration, Jefferson, AR 72079-9502, USA.
出版信息
J AOAC Int. 1996 Mar-Apr;79(2):389-96.
A liquid chromatographic (LC) method with fluorescence detection was developed for analysis of amoxicillin in catfish and salmon tissues. The tissue was extracted with phosphate buffer (pH 4.5), followed by trichloroacetic acid (TCA) precipitation of proteins and solid-phase (C18) extraction. Trace amounts of nonpolar interfering substances present after solid-phase extraction were removed by ether liquid-liquid extraction. The extract was reacted with formaldehyde and TCA at 100 degrees C for 30 min. A fluorescent derivative was extracted with ether, concentrated, and analyzed by reversed-phase LC with fluorescence detection. Average recoveries of amoxicillin spiked at 2.5-20 ppb were > 80% for catfish and > 75% for salmon muscle tissue, with coefficients of variation of < 6%. Limits of detection (LOD) and quantitation (LOQ) for catfish tissue were 0.5 and 1.2 ppb, respectively. LOD and LOQ for salmon muscle tissue were 0.8 and 2.0 ppb, respectively.
建立了一种带荧光检测的液相色谱（LC）方法，用于分析鲶鱼和三文鱼组织中的阿莫西林。组织先用磷酸盐缓冲液（pH 4.5）提取，然后用三氯乙酸（TCA）沉淀蛋白质并进行固相（C18）萃取。固相萃取后存在的痕量非极性干扰物质通过乙醚液 - 液萃取去除。提取物在100℃下与甲醛和TCA反应30分钟。用乙醚萃取荧光衍生物，浓缩后通过带荧光检测的反相LC进行分析。在鲶鱼中添加浓度为2.5 - 20 ppb的阿莫西林时，平均回收率> 80%，在三文鱼肌肉组织中> 75%，变异系数< 6%。鲶鱼组织的检测限（LOD）和定量限（LOQ）分别为0.5和1.2 ppb。三文鱼肌肉组织的LOD和LOQ分别为0.8和2.0 ppb。
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