HPLC法测定复方替米考星颗粒中有效成份含量

Determination of active ingredient in compound tilmicosin particle by HPLC

关键词:  替米考星  磺胺二甲氧嘧啶  甲氧苄啶  高效液相色谱法  含量

Key words:  tilmicosin  sulfamethazine  trimethoprim  HPLC  content

摘要:

[摘 要] 方法：采用HPLC法同时测定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5 μm），流动相为磷酸二丁胺缓冲液-乙腈-四氢呋喃-水（25：115：55：805），检测波长为280 nm，流速为1.0 mL/min。结果：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。替米考星在6.25～125 μg/mL浓度范围内线性关系良好(R2 =0.996)，磺胺二甲氧嘧啶在3.125～62.5 μg/mL浓度范围内线性关系良好(R2 =0.996)，甲氧苄啶在0.625～12.5 μg/mL浓度范围内线性关系良好(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%。结论：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。

Abstract:

Abstract: An HPLC method has been developed determine tilmicosin、sulfamethazine and trimethoprim. Eclipse XCB-C18 column (250mm×4.6mm,5μm) was used. The mobile phase was 2-butylamine phosphate buffer -acetonitrile-tetrahydrofuran-water（25：115：55：805）at the wavelength of 280 nm.The flow rate was 1.0 mL/min. The peaks in order of trimethoprim, sulfamethazine, tilmicosin trans-structure and tilmicosin cis-structure. Theoretical plate numbers were 7963, 15714, 3282, 8701. The separation between the two peaks, respectively 24.29,3.92,2.91. Tailing factor were 0.92, 0.90, 0.97, 0.94. The linear relationship of tilmicosin was good in range of 6.25~125 μg/mL (R2 =0.996); The linear relationship of sulfamethazine was good in range of 3.125~62.5 μg/mL (R2 =0.996); The linear relationship of trimethoprim was good in range of 0.625~12.5 μg/mL (R2 =0.999). The average recoveries were 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 compound tilmicosin content of particles in three kinds of ingredients.