化学原料药中19种金属杂质的检测研究

目的:以格列齐特为研究对象,建立化学原料药中19种金属杂质的测定方法。方法:采用电感耦合等离子体发射光谱法,供试品经微波消解前处理后测定。为克服各元素之间的光谱干扰,且保证检测灵敏度,将所有元素分为3个系统,确定合适的发射谱线和观测模式,同时对等离子参数进行优化。结果:在一定的浓度范围内,各元素谱线的发射强度均与浓度呈良好的线性关系,相关系数均大于0.999,加样回收率为76.6%～123.0%,检测限均满足测定的要求。结论:该方法专属性好,灵敏度高,准确快捷,可替代传统的重金属检查法,用于化学原料药中金属杂质的测定。

Study on determination of nineteen elemental impurities in chemical bulk drug

Objective:To establish a method for determination of nineteen elemental impurities in chemical bulk drugs by choosing gliclazide as research object.Methods:Elemental impurities were determined by inductively coupled plasma-atomic emission spectrometry,using microwave digestion for sample pretreatment.All elements were divided into three systems in order to overcome the spectral interference between them and guarantee the sensitivity of determination.The appropriate emission lines and the observation mode of every element were determined,and the plasma parameters were optimized.Results:The emission intensity and the concentration of every elements showed a good linear relationship in certain concentration range,and the correlation coefficients were all greater than 0.999.The recoveries were from 76.6%-123.0%,and the detection limits all met the requirements of determination.Conclusion:The method is specific,sensitive,accurate and rapid,and can be used for the determination of elemental impurities in chemical bulk drugs as a replacement to the traditional method for heavy metals.