4—氨基吡啶有关物质方法研究

Determination of Related Substances in 4-Aminopyridine

建立高效液相色谱法测定4—氨基吡啶的有关物质。色谱柱为Waters symmetry C_(18)(4.6 mm×250 mm,5μm);流动相A为0.02 mol/L磷酸二氢钾+0.1 mol/L庚烷磺酸钠(磷酸调pH=3.0),流动相B为70%乙腈水,梯度洗脱;体积流量1.0 mL/min;检测波长为262 nm;进样体积为20μL;柱温为40℃。在选定的条件下,4—氨基吡啶与已知杂质A、B、C分离度良好;杂质A、B、C、4—氨基吡啶分别在0.1021~1.0210,0.1165~1.1650,0.1041~1.0410,0.1067~1.0670μg/mL质量浓度范围内线性关系良好;杂质A、B、C定量限分别为0.51,0.58,0.52,0.53 ng/mL;重复性和回收率结果良好。结论:该法专属、准确、易于操作,适用于4—氨基吡啶有关物质的测定。

To establish a method to the determination the related substances of 4-Aminopyridine,the chromatographic column was Waters symmetry C_(18)(4.6 mm×250 mm,5μm),and the mobile phase A was 0.02 mol/L potassium dihydrogen phosphate and 0.1 mol/L sodium heptanesulfonate(adjusted pH=3.0 with phosphoric acid).The mobile phase B was 70%acetonitrile water with gradient elution;the flow rate was 1.0 mL/min.The detection wavelength was 262 nm;the injection volume was 20μL;the column temperature was 40℃.Under the described chromatographic condition,4-aminopyridine was completed separated from the impuritie A,B and C.The linear range of impuritie A,B,C and 4-aminopyridine were 0.1021~1.0210,0.1165~1.1650,0.1041~1.0410,0.1067~1.0670μg/mL,respectively.The LOQ of impurities A,B and C were 0.51,0.58,0.52 and 0.53 ng/mL,respectively.The repeatability and recovery were suitable.The method is specific,accurate and suitable for the analysising the related substances in 4-aminopyridine.