Ashok Sigala, Varma M Satish, Swaminathan Srinivasan
Dr. Reddy's Laboratories Ltd., Integrated Product Development, Bachupally, Hyderabad 500 072, India.
J Chromatogr Sci. 2012 Oct;50(9):799-802. doi: 10.1093/chromsci/bms073. Epub 2012 Jun 24.
High-performance liquid chromatography enantioseparation of aliskiren hemifumarate was accomplished on an immobilized-type Chiralpak IC chiral stationary phase under both polar organic and reversed-phase modes. A simple analytical method was developed and validated using a mixture of acetonitrile-n-butylamine 100:0.1 (v/v/) as a mobile phase with a flow rate maintained at 1.0 mL/min. Ultraviolet detection was carried out at 228 nm. Resolution between the two enantiomers was greater than 3.0. This method was capable of detecting the R-isomer to a level of 0.2 μg/mL. The method was validated as per International Conference on Harmonization guidelines and found to be robust. The method is very useful for routine evaluation of the quality of aliskiren hemifumarate in bulk drug manufacturing units.
在固定化型Chiralpak IC手性固定相上，在极性有机模式和反相模式下均实现了阿利吉仑半富马酸盐的高效液相色谱对映体分离。开发了一种简单的分析方法，并使用乙腈 - 正丁胺100:0.1（v/v/）的混合物作为流动相进行验证，流速保持在1.0 mL/min。在228 nm处进行紫外检测。两种对映体之间的分离度大于3.0。该方法能够检测到R - 异构体的水平为0.2 μg/mL。该方法按照国际协调会议指南进行了验证，结果表明该方法具有稳健性。该方法对于原料药生产单位中阿利吉仑半富马酸盐质量的常规评估非常有用。
