利伐沙班原料药中重金属镍残留量的检测方法与评价

Detection Method and Evaluation of Heavy Metal Nickel Residues in Rivaroxaban API

目的:建立利伐沙班原料药中金属催化剂镍残留的两种测定方法,并对不同方法进行比较分析。方法:方法一采用石墨炉原子吸收分光光度法;方法二采用电感耦合等离子体质谱法。结果:方法一在10~100μg·L^-1范围内线性良好,最低检出浓度为1.9μg·L^-1,方法检测限为0.2μg·g^-1,加标回收率平均为112%;方法二在0.5~20μg·L^-1范围内线性良好,最低检出浓度为0.056μg·L^-1,方法检测限为0.007μg·g^-1,加标回收率平均为97.9%。结论:6批样品的检验结果表明,两种方法对结果的测量无明显差异,但电感耦合等离子体质谱法具有分析速度快、检测限更低、灵敏度高以及可多种元素同时测定等优点,在重金属痕量分析检测方面更具优势。

Objective:To establish and compare two methods for the determination of nickel residues of metal catalyst in rivaroxaban API.Methods:The method one used graphite furnace atomic absorption spectrophotometry;the method two used inductively coupled plasma mass spectrometry.Results:The method one had a good linearity in the range of 10 to 100μg·L^-1,the minimum detection concentration was 1.9μg·L^-1,the detection limit of this method is 0.2μg·g^-1 and the average recoveries were 112%.The method two had a good linearity in the range of 0.5 to 20μg·L^-1,the minimum detection concentration was 0.056μg·L^-1,the detection limit of this method was 0.007μg·g^-1 and the average recoveries were 97.9%.Conclusion:The inspection results of 6 batches of samples show that there is no significant difference between the two methods,but the inductively coupled plasma mass spectrometry has the advantages of fast analysis speed,lower detection limit,high sensitivity,and simultaneous determination of multiple elements,so it has more advantages in the analysis and detection of heavy metal traces.