摘要
目的：建立凝血酶抑制剂阿加曲班原料药中催化剂钯的残留量测定方法。方法采用石墨炉原子吸收分光光度法测定阿加曲班中钯的残留量。试验条件：光源为钯空心阴极灯,波长247.6 nm,狭缝0.5 nm,灯电流10 mA,燃烧器高度2 mm,石墨管以横向加热方式,氩气压力0.4 MPa,进样体积20μL,背景校正D2,石墨炉程序升温。结果钯在0.015－0.2μg·mL-1范围内与吸光度呈良好的线性关系（r=0.9996）；检出限为0.00057μg·mL-1；特征浓度为0.00107μg·mL-1；平均回收率为99.8%；RSD 为4.08%（n=9）。结论该方法经方法学验证可用于阿加曲班原料药中痕量钯含量的测定,可为该原料药质量标准的完善提供参考。
Objective To establish a method for the content determination of palladium catalyst residue in thrombin inhibitor argatroban bulk drug.Methods Graphite furnace atomic absorption spectrometry （AAS）method was used to determine palladium residue content in argatroban.Test conditions were as follows.The palladium hollow cathode lamp was used for light source.The detection wavelength was 247.6 nm,and the slit was 0.5 nm.The lamp current was 10 mA,and the burner height was 2 mm with transverse heating graphite tube.The argon pressure was 0.4 MPa.The injection volume was 20μL with background correction D2.The temperature program was used for graphite furnace.Results It showed a good linear relationship within the concentration range of 0.0 1 5-0.2 μg · mL-1 （r=0.9 9 9 6 ）. The detection limit and the characteristic concentration were 0.00057 μg · mL-1 and 0.00107 μg · mL-1 , respectively.The average recovery was 99.8%,with RSD of 4.08% （n=9）.Conclusion This method could be used for the determination of the trace palladium content in argatroban bulk drug after methodology verification,and could provide reference for improving quality standard of the raw material medicine.
出处
《中国药事》
CAS
2014年第9期1018-1020,共3页
Chinese Pharmaceutical Affairs
