HPLC法检测阿托伐他汀钙有关物质的含量及光学纯度

目的: 检测阿托伐他汀钙原料有关物质的含量及光学纯度。 方法: 采用反相高效液相色谱法,测定阿托伐他汀钙有关物质的含量。色谱条件:色谱柱为Kromasil C₁₈(4.6 mm×250 mm,5 μm),流动相:乙腈-四氢呋喃-0.05 mol·L^-1枸橼酸铵溶液 (0.05 mol·L^-1枸橼酸溶液用氨水调节pH至4.0) (42∶ 3∶ 55);同时采用正相高效液相色谱法测定阿托伐他汀钙的光学纯度,色谱柱为CHIRALPAK AD-H(4.6 mm×250 mm,5 μm),流动相:正己烷-乙醇-冰醋酸(90∶ 10∶ 0.3),检测波长均为244 nm,柱温为35 ℃。 结果: 检测3批阿托伐他汀钙样品中双胺、脱氟体、非对映异构体和对映异构体含量分别为0.05%~0.09%,0.16%~0.20%,0.03%~0.05%,0.18%~0.24%。 结论: 该方法简单、稳定、可靠、专属性强,可用于阿托伐他汀钙有关物质的检测,为阿托伐他汀钙的质量控制提供了新方法。

Objective: To establish an HPLC method for the determination of the related substances and enantiomeric purity of atorvastatin calcium. Methods: The liquid chromatographic procedures in the tests for related compounds was performed on the Kromasil C₁₈ column(4.6 mm×250 mm,5 μm) with acetonitrile-tetrahydrofuran(THF)-ammonium citrate pH 4.0 (42∶ 3∶ 55) as mobile phase.The liquid chromatographic procedures for enantiomeric purity was performed on the CHIRALPAK AD-H column(4.6 mm×250 mm,5 μm) with hexane-dehydrated alcohol-glacial acetic acid (90∶ 10∶ 0.3) as mobile phase.The detection wavelength was 244 nm,the column temperature was 35 ℃. Results: The proposed method was applied to the determination of impurities and was found to contain 0.05%-0.09%,0.16%-0.20%,0.03%-0.05%,0.18%-0.24% of the diamine-atorvastatin,desfluoro-atorvastatin,diastereomer-atorvastatin and enantiomer-atorvastatin. Conclusion: The method is simple,selectivity and reliable,which provide new ways for the quality control of atorvastatin calcium.