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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 the simultaneous determination of cefalexin and trimethoprim in capsules by ultra performance liquid chromatography (UPLC) and to compare with the results of the national standard drug method. Methods Waters BEH C18 column (100 mm × 2.1 mm, 1.7 μm) was used as the mobile phase with 0.02 mol / L sodium dihydrogen phosphate (pH = 3.0 with phosphoric acid) -acetonitrile (85:15, V / V) The flow rate was 0.25 ml / min, the column temperature was 30 ℃, the detection wavelength was 235 nm and the injection volume was 5μl. The contents of cephalexin and trimethoprim in capsules were determined by UPLC. Results The contents of cefalexin and trimethoprim were 0.005 g ~ 0.471 g and 0.001 g ~ 0.098 g, respectively. The correlation coefficients (r) were 0.999 0 and 0.999 4, respectively. The average recoveries were 99.6% and 99.8%, respectively. The relative standard deviations (RSDs) were 0.3% and 0.4% respectively. 4 batches of samples using the proposed method of determination of the results of the national standard test method and the relative average deviation ≤ 0.4%. Conclusion The method is rapid, sensitive, accurate and reproducible. The method is comparable to the standard method of the national drug standard and can be used for the simultaneous determination of cefalexin and trimethoprim in capsules.