HPLC法测定复方替米考星颗粒中有效成份含量

采用HPLC法同时测定了复方替米考星颗粒中替米考星、磺胺二甲氧嘧啶及甲氧苄啶的含量。色谱柱为Eclipse XCB-C18(250 mm×4.6 mm,粒径5μm),流动相为磷酸二丁胺缓冲液-乙腈-四氢呋喃-水(25∶115∶55∶805),检测波长280 nm,流速1.0 mL/min。出峰顺序为甲氧苄啶、磺胺二甲氧嘧啶、替米考星反式结构、替米考星顺式结构,理论塔板数分别为7963、15714、3282、8701。两峰之间的分离度分别为24.29、3.92、2.91;拖尾因子分别为0.92、0.90、0.97、0.94。替米考星、磺胺二甲氧嘧啶、甲氧苄啶的浓度线性范围分别是6.25～125μg/mL(R2=0.996),3.125～62.5μg/mL(R2=0.996),0.625～12.5μg/mL(R2=0.999);平均回收率分别为99.17%、99.06%和99.39%;RSD分别为0.8%、0.9%和0.9%。该法快速、灵敏、准确,适用于同时测定复方替米考星颗粒中三种成份的含量。

Determination of active ingredient in compound tilmicosin particle by HPLC

An HPLC method has been developed to determine tilmicosin,sulfamethazine and trimethoprim.Eclipse XCB-C18 column（250 mm×4.6 mm,5 μm） was used.The mobile phase was 2-butylamine phosphate buffer-acetonitrile-tetrahydrofuran-water（25∶115∶55∶805）,the wavelength was 280 nm,the flow rate was 1.0 mL/min.The peaks in order was trimethoprim,sulfamethazine,tilmicosin trans-structure and tilmicosin cis-structure.Theoretical plate numbers was 7963,15714,3282,8701.The separation between two peaks was 24.29,3.92,2.91 respectively.Tailing factor was 0.92,0.90,0.97,0.94.The linear concentration range of tilmicosin,sulfamethazine and trimethoprim was 6.25～125 μg/mL（R^2=0.996）,3.125～62.5 μg/mL（R^2=0.996）,0.625～12.5 μg/mL（R^2=0.999）;the average recoveries was 99.17%,99.06% and 99.39% with RSD of 0.8%,0.9% and 0.9%.This method is rapid,sensitive and accurate,suitable for simultaneous determination of three ingredients in compound tilmicosin particles.