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目的:建立水产品中泰乐菌素残留量的高效液相色谱测定方法。方法:样品在碱性条件下用乙酸乙酯提取,提取液旋转蒸干后,经正己烷脱脂,SCX柱固相萃取净化,乙腈与磷酸盐缓冲液为流动相梯度洗脱,外标法定量。结果:泰乐菌素在0.050μg/ml~5.00μg/ml内呈良好线性关系,相关系数r=0.9998。检出限为30μg/kg,定量限为100μg/kg。在50μg/kg~500μg/kg添加水平下回收率为72.4%~106%,相对标准偏差均小于10%。结论:该方法的灵敏度和重复性均满足水产品中泰乐菌素药物残留量检测需要。
Objective: To establish a method for the determination of tylosin residues in aquatic products by high performance liquid chromatography. Methods: The sample was extracted with ethyl acetate under alkaline conditions. The extract was rotary evaporated to dryness. The sample was degreased with n-hexane, purified by SCX column and eluted with mobile phase of acetonitrile and phosphate buffer. . Results: Tylosin showed good linearity in the range of 0.050μg / ml ~ 5.00μg / ml with a correlation coefficient of 0.9998. The detection limit was 30μg / kg, the limit of quantification was 100μg / kg. The recoveries ranged from 72.4% to 106% at 50μg / kg ~ 500μg / kg with relative standard deviations less than 10%. Conclusion: The sensitivity and repeatability of this method all meet the need of tylosin drug residues detection in aquatic products.