摘要
目的建立测定瑞舒伐他汀钙合成中间物料(4 R-顺式)-6-醛基-2,2-二甲基-1,3-二氧己环-4-乙酸叔丁酯中乙醛、乙醇、二甲硫醚、甲苯4种有机溶剂残留的顶空气相色谱法。方法色谱柱为以6%氰丙基苯基-94%二甲基聚硅氧烷为固定相的Rtx-624毛细管柱(60 m×0.25 mm,1.4μm),程序升温,火焰离子化检测器,检测器温度为250℃,进样口温度为200℃,分流比为30∶1,载气为氮气,顶空瓶平衡温度为90℃,顶空瓶平衡时间为30 min,定量环温度为120℃,传输线温度为130℃,进样量为1 m L;GCMS Solution 2.71工作站,电子轰击(ESI)离子源,离子源温度230℃,传输线温度250℃;质量扫描范围m/z为45~550。结果乙醛、乙醇、二甲硫醚及甲苯与各相邻色谱峰能完全分离,质量浓度分别在80.04~800.36μg/mL、103.94~1039.44μg/mL、19.27~192.68μg/mL、17.97~179.72μg/m L范围内与峰面积线性关系良好(R2均大于0.995);平均回收率分别为92.73%,91.75%,88.45%,86.89%,RSD分别为2.33%,3.19%,2.57%,3.62%(n=9)。结论该方法操作简单,准确度高,灵敏度好,可用于检测瑞舒伐他汀钙合成中间物料有机溶剂的残留量,可为该物料的质量控制提供参考。
Objective To establish a headspace gas chromatography method for the determination of acetaldehyde,ethanol,dimethyl sulfide and toluene in the synthetic intermediate materials(4 R-cis)-6-aldehyde-2,2-dimethyl-1,3-dioxane-4-butyl acetate of rosuvastatin calcium.Methods Gas chromatography(GC)was performed with Rtx-624 capillary column(60 m×0.25 mm,1.4μm)with6%cyanopropylphenyl-94%dimethylpolysiloxane as stationary phase and programmed heating,the detector was flame ionization detector(FID)with temperature of 250℃,the temperature of injection port was 200℃,the split ratio was 30∶1,the carrier gas was nitrogen,the equilibrium temperature of headspace bottle was 90℃,the equilibrium time of headspace bottle was 30 min,the temperature of quantitative loop was 120℃,the temperature of transmission line was 130℃,and the injection volume was 1 m L.GCMS solution 2.71 workstation was adopted with electron bombardment(ESI)ion source,the temperature of ion source was 230℃,the temperature of transmission line was 250℃,and the mass scanning range m/z was 45-550.Results Acetaldehyde,ethanol,dimethyl sulfide and toluene were completely separated from the adjacent peaks,and their linear ranges were 80.04-800.36μg/m L,103.94-1039.44μg/m L,19.27-192.68μg/m L,17.97-179.72μg/m L(R2>0.995),respectively.The average recoveries of acetaldehyde,ethanol,dimethyl sulfide and toluene were 92.73%,91.75%,88.45%,86.89%with RSDs of 2.33%,3.19%,2.57%,3.62%(n=9),respectively.Conclusion The method is simple,accurate and sensitive,which can be used for the determination of residual organic solvents in the synthetic intermediate materials of rosuvastatin calcium and provide a reference for the quality control of the materials.
作者
斯智萍
徐世芳
SI Zhiping;XU Shifang(Zhejiang Helixinjian Pharmaceutical Co.,Ltd.,Huzhou,Zhejiang,China 313000;Hangzhou Medical College,Hangzhou,Zhejiang,China 310013)
出处
《中国药业》
CAS
2021年第14期66-69,共4页
China Pharmaceuticals
关键词
顶空气相色谱法
瑞舒伐他汀钙
合成中间物料
残留有机溶剂
headspace gas chromatography
rosuvastatin calcium
synthetic intermediate materials
residual organic solvents
