盐酸艾咪朵尔相关物质的分离与含量测定

Separation and content determination of the related substances of imidol hydrochloride by RP-HPLC

目的建立RP-HPLC法分离测定盐酸艾咪朵尔相关物质。方法色谱柱为Agilent TC-C18柱(150 mm×4.6 mm,5μm),柱温35℃,以乙腈-甲酸水溶液(甲酸-水体积比0.3∶100)为流动相进行梯度洗脱,流速为1.0 mL.m in-1,检测波长254 nm。结果确定了盐酸艾咪朵尔合成中可能引入的杂质A、B、C和盐酸艾咪朵尔的出峰位置,在盐酸艾咪朵尔原料中,杂质A、B、C的含量质量分数均小于0.1%。结论采用杂质外标对照法较质量分数1%主成分自身对照法更能直接反映盐酸艾咪朵尔中有关物质的情况。

Objective To develop an HPLC method for the separation of imidol hydrochloride and its known related compounds.Methods The analysis was conducted on Agilent TC-C18 column（150 mm × 4.6 mm,5 μm）with a mobile phase of acetonitrile-water（V∶V=0.3∶100）by gradient elution at a flow rate of 1.0 mL·min-1.The detection wavelength was set at 254 nm.Results The retention time of imidol hydrochloride and relevant impurities A,B and C were determined.The impurities A,B and C had been found with levels below 0.1% in the raw material.Conclusions The external standard method of impurities can provide more satisfactory results than the one with 1% reference solution corresponding impurities in both qualification and quantization for the impurities in imidol hydrochloride with sufficient accuracy,specificity and sensitivity.