高效液相色谱法同时检测水产品中螺旋霉素与泰乐菌素药物残留

Simultaneous Determination of Residual Spiramycin and Tylosin in Aquatic Products by HPLC

建立了同时检测水产品中螺旋霉素与泰乐菌素药物残留的分析方法。在碱性条件下采用乙酸乙酯提取,提取液挥干后溶于酸性缓冲液中,经正己烷去脂、HLB SPE小柱净化后,采用高效液相色谱进行分析。采用Meck Purospher STAR RP18色谱柱(250 mm×4.6 mm,5μm)及乙腈和pH 2.5磷酸缓冲溶液的混合液作梯度淋洗进行分离。分别在232 nm及287 nm对螺旋霉素及泰乐菌素进行紫外检测。方法在1-200 ng之间呈线性相关,相关系数在0.999 8以上,平均回收率为82.2%-89.0%,相对标准偏差为6.24%-9.83%,对螺旋霉素、泰乐菌素的检出限分别为0.005 4 mg.kg-1与0.031 mg.kg-1。

Residual spiramycin and tylosin in sample were extracted with ethyl acetate from phosphate buffer solution of pH 8, and defatted with n-hexane. The sample solution in the phosphate buffer was then purified by passing through HLB column. The objective analytes on the column were eluted with a solution of triethylamine in methanol, The eluate was blown with nitrogen to dryness at 40 ℃, and residue was taken up with the mobile phase and ready for HPLC deterrnination. The Meck Purospher STAR RP18 column （250 mm×4.6 mm, 5 μm） was used as chromatographic column, and gradient elution with mixed solutions of acetonitrile and phosphate buffer solution （pH 2.5） in different ratio was applied in the separation. UV-detections were made at 232 nm for spiramycin and at 287 nm for tylosin. Linear relationships between peak area and concentration of both the compounds were found in the range within 200 ng （r=0. 999 9）. Detection limits for spiramycin and tylosin were found to be 0. 005 4 mg· kg^-1 and 0. 031 mg· kg^-1 espectively. Tests for precision and recovery were made, and the results obtained were in the ranges of 6.24%-9.83% and 82. 2%-89.0% respectively.