高效液相色谱法检测泰乐菌素残留

Determination of Residual Tylosin by HPLC

建立了酵母培养物和饲用酶制剂中残留泰乐菌素的高效液相色谱检测方法。采用Diamonsil(钻石)C18(5μm,150mm×4.6mm)反相色谱柱,利用正己烷在索氏提取器中脱脂,以甲醇为提取液,流动相为0.04mol·L-1磷酸盐缓冲溶液(pH=2.4)∶乙腈,采用等度洗脱,流速为1mL·min-1,用紫外检测器检测,检测波长为285nm,进样量20μL。泰乐菌素的检出限为0.31mg·mL-1,在0.75～50mg·mL-1范围内线性相关系数R2=0.9993;在10mg·mL-1、50mg·mL-1、100mg·mL-1添加水平的回收率为47.25%～75.92%,相对标准偏差为2.45%～8.53%。

A high performance liquid chromatographic（HPLC）method was developed for determination of residual tylosin in yeast culture and feed enzyme preparation.The method used reversed phase column of Diamonsil C18（5 μm,150 mm×4.6 mm i.d.）as analysis column.The samples were degreased with n-hexane in Soxhlet extractor.The extraction solution was methanol and the mobile phase was acetonitrile-0.04 mol·L-1 phosphate buffer（pH=2.4）with isocratic elution,the flow rate was 1 mL·min-1.The detection wavelength was 285 nm and the injection volume was 20 μL.The limit of detection was 0.31 mg·L-1.The linear correlation coefficient of 0.9993 was obtained between 0.7550 mg·L-1.Overall recoveries were from 47.25% to 75.92% and the relative standard deviations were between 2.45% to 8.53%.