HPLC法测定盐酸氨丙啉的含量及对杂质2-甲基吡啶进行检查

Determination of amprolium hydrochloride and 2-picoline impurity by HPLC

采用高效液相色谱法测定盐酸氨丙啉的含量及对杂质2-甲基吡啶进行检查。用WatersXTerraTMRPC18色谱柱,以乙腈-甲醇-庚烷磺酸钠溶液(将12g的1-庚烷磺酸钠溶于1000mL水中,加24mL冰醋酸,6mL的三乙胺制得)(5∶35∶60)为流动相,用紫外检测器于254nm处检测,柱温30℃,流速1.0mL/min。在该条件下盐酸氨丙啉和2-甲基吡啶的分离度很好,盐酸氨丙啉浓度在0.05～0.50mg/mL范围内,其色谱峰面积与浓度呈良好的线性关系,回归方程为y=3.07×107x-3.90×104,r=0.9999,RSD=0.76%。该法适用于盐酸氨丙啉原料药的质量控制。

A HPLC method for determination of amprolium hydrochloride and 2-picoline impurity was established with Waters XTerra TM RP_ 18 column (3.9 mm×150 mm,5 μm) and acetonitrile-methanol-solution of sodium 1-heptanesulfonate (5∶35∶60 ) as mobile phase. The wavelength of UV detector was set at 254 nm. The column temperature was 30 ℃. The flow rate was 1.0 mL/min. The calibration curve was linear in the range of 0.05~0.50 mg/mL for amprolium hydrochloride and the regression equation was y =3.07×107x-3.90×104, r=0.999 9. This method is simple, rapid, accurate and suitable for the quality control of the drug.