HPLC法测定甲硫酸新斯的明原料药的有关物质

Determination of Related Substances in Neostigmine Metilsulfate by HPLC

建立了HPLC测定原料药甲硫酸新斯的明中有关物质的方法。采用Kromasil 100(250 mm×4.6 mm,5 mm)色谱柱,以辛烷磺酸钠缓冲液为流动相A,以辛烷磺酸钠缓冲液-乙腈(30:70)为流动相B,采用梯度洗脱法,设流速为1.0 mL/min,柱温设为25.0℃,检测的波长为210 nm,进样的体积为20μL。甲硫酸新斯的明对照品色谱峰与三个已知杂质峰均能良好分离,甲硫酸新斯的明对照品及已知杂质在考察的浓度范围内有良好的线性关系,甲硫酸新斯的明、杂质A、杂质B与杂质C的检测限分别为0.016 mg·mL^(-1)、0.022 mg·mL^(-1)、0.004 mg·mL^(-1)、0.007 mg·mL^(-1)。该方法灵敏度高,专属性强,可用于甲硫酸新斯的明原料药的有关物质测定。

HPLC method was established to determine related substances in Neostigmine Metilsulfate.The determination was performed on a Kromasil 100(250 mm×4.6 mm,5 mm)column.The mobile phase consisted of sodium octane sulfonate buffer(mobile phase A)and sodium octane sulfonate buffer-acetonitrile(30:70)mobile phase B with gradient elution.The flow rate was 1.0 mL·min^(-1),column temperature wae maintained at 25.0℃,the detection wavelength was 210 nm,and injection volume was 20μL.The peaks of the Neostigmine Metilsulfate were well separated from the peaks of the three known impurities within the concentration range investigated,and the detection limits of Neostigmine Metilsulfate,impurity A,impurity B and impurity C were 0.016,0.022,0.004,and 0.007 mg·mL^(-1) respectively.This method has high sensitivity and strong specificity,and can be used for the determination of neostigmine methylsulfate.