12种兽药中非法添加甲氧苄啶的HPLC-PDA检查方法的建立

Determination of Trimethoprim in the 12 Kinds of Verterinary Drugs by HPLC-PDA

采用十八烷基键合硅胶为填充剂，以0．02 mol／L磷酸二氢钾溶液－甲醇（73∶27，V／V）为流动相，建立了测定12种兽药中非法添加甲氧苄啶的HP LC－P DA法，并采用峰纯度检查和光谱相似度检查辅助对照品比对方法，对非法添加药物进行确证。在此液相条件下，对7种兽药粉散剂和5种注射液药物，进行添加回收试验和检测限的测定。结果显示，甲氧苄啶在粉剂中三个浓度（1％、5％、10％）添加回收率为74．6％～115．0％，RSD为0．1％～7．6％，在注射液中三个浓度（0．5％、1％、2％）的添加回收率为87．0％～119．7％，RSD为0．9％～4．1％。甲氧苄啶在各制剂中的检测限为0．5 mg／g（0．25 mg／mL）。改变试验条件后对峰纯度指示、光谱相似度进行考察，仍能满足要求。

C18 column was used, mobile phase was phosphate buffer and methnol （ 73 ∶ 27, V/V ） , and established a method for determination of trimethoprim in the 12 kinds of veterinary drugs by HPLC-PDA . Peak purity test and spectrum similar test were helped to identify the trimethoprim.Under this liquid condition, the test of added recycling,the determination of detection limit were operated.Results showed that the added recycling rate of TMP in the veterinary powder under three levels （ 1%, 5%, 10%） were 74. 6%~115. 0%, the RSD were 0.1%~7.6%. and injection under three levels （0.5%, 1%, 2%） were 87.0%~119.7%, the RSD were 0.9%~4.1%. Detection limit of trimethoprim in the preparation has got by this method was 0.5 mg/g （0.25 mg/mL）. Changing the test conditions,the purity test,spectral similarity can meet the requirements.