Coyne Rosie, Bergh Øivind, Samuelsen Ole Bent
Department of Aquaculture, Institute of Marine Research, P.O. Box 1870, Nordnes, N-5817 Bergen, Norway.
J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Oct 25;810(2):325-8. doi: 10.1016/j.jchromb.2004.08.015.
A one-step simple and rapid high performance liquid chromatography (HPLC) method was developed for the determination of oxytetracycline (OTC) in fish tissue. The method involves liquid extraction of muscle tissue, precipitation of proteins and reversed phase HPLC analysis with spectrophotometric detection. The limit of quantitation of OTC in spiked fish muscle was 0.04 microg/g and the method showed high linearity (r(2) = >0.999) in the working range of 0.04-2 microg/g. The precision (%R.S.D.) was between 1.9 and 7.5% for the concentration range 0.04-1.0 microg/g and there was no significant difference between the concentrations determined on three different test days for all four spiked concentrations. The percentage recovery over the spiked concentration range 0.04-1.0 microg/g was consistently within a narrow range of 33-35%. While the method had the advantage of high precision, sensitivity and linearity, the method's additional salient advantages included high sample through-put (60 individual preparations per day) and minimum amount of consumables, time and labour required to perform the analysis. The method was successfully applied to a pharmacokinetic study.
建立了一种一步简单快速的高效液相色谱（HPLC）法，用于测定鱼组织中的土霉素（OTC）。该方法包括肌肉组织的液液萃取、蛋白质沉淀以及采用分光光度检测的反相HPLC分析。加标鱼肌肉中土霉素的定量限为0.04μg/g，该方法在0.04 - 2μg/g的工作范围内具有高线性（r(2) =>0.999）。对于0.04 - 1.0μg/g的浓度范围，精密度（%R.S.D.）在1.9%至7.5%之间，对于所有四个加标浓度，在三个不同测试日测定的浓度之间无显著差异。在0.04 - 1.0μg/g的加标浓度范围内，回收率百分比始终在33 - 35%的窄范围内。该方法具有高精度、高灵敏度和高线性的优点，其额外的显著优点包括高样品通量（每天60个单独制剂）以及进行分析所需的耗材、时间和劳动力最少。该方法已成功应用于一项药代动力学研究。
