超高效液相色谱法测定胶囊中头孢氨苄和甲氧苄啶的含量

Determination of cefalexin and trimethoprim in capsules by UPLC

目的建立超高效液相色谱法(UPLC)同时测定胶囊中头孢氨苄与甲氧苄啶含量的方法,并与国家药品标准法测得的结果进行对比。方法采用Waters BEH C18色谱柱(100 mm×2.1 mm,1.7μm),以0.02 mol/L磷酸二氢钠(用磷酸调p H值至3.0)-乙腈(85∶15,V/V)为流动相,流速为0.25 ml/min,柱温为30℃,检测波长为235 nm,进样体积为5μl,通过UPLC对胶囊中头孢氨苄与甲氧苄啶的含量进行测定。结果头孢氨苄、甲氧苄啶的含量分别为0.005 g^0.471 g、0.001 g^0.098 g时,线性关系良好,相关系数(r)分别为0.999 0、0.999 4。方法的平均回收率分别为99.6%、99.8%,相对标准偏差(RSD)分别为0.3%、0.4%。4批样品采用拟定方法的测定结果与国家药品标准法测得结果的相对平均偏差≤0.4%。结论此方法快速灵敏,准确可靠,重复性好,且与国家药品标准方法检验结果相当,可用于胶囊中的头孢氨苄与甲氧苄啶含量的同时测定。

Objective To establish a method for simultaneous determination of cefalexin and trimethoprim in capsules by ultra performance liquid chromatography（ UPLC）,and the results were compare with the national statutory testing results. Methods The separation column was Waters BEH C18column（ 100 mm × 2. 1 mm,1. 7 μm）,and the mobile phase was 0. 02 mol / L sodium dihydrogen phosphate（ p H 3. 0）- acetonitrile（ 85∶15） with flow rate of 0. 25 ml / min. The column temperature was set at 30 ℃,detection wavelength was 235 nm and the injection volume was 5 μl. Cefalexin and trimethoprim in capsules determined determined by UPLC. Results When the content of cefalexin and trimethoprim were 0. 005 g- 0. 471 g,0. 001 g-0. 098 g,the linear relationship was good with correlation coefficient of 0. 999 0 and 0. 999 4,respectively. The average recoveries were 99. 6% and 99. 8%,respectively and RSD was 0. 3% and 0. 4%,respectively. Compared the determination results of 4 batches of samples determined by the proposed method with statutory method,the relative average deviation was not more than 0. 4%. Conclusion The method is rapid,sensitive,accurate with good reproducibility,and the results were consistent with the statutory method. So it can be used for determination of cefalexin and trimethoprim in capsules.