Assay method for quality control and stability studies of a new antimalarial agent (CDRI 99/411)  

作　　者：Kiran Khandelwal Shakti Deep Pachauri Sofa Zaidi Pankaj Dwivedi Ashok Kumar Sharma Chandan Singh Anil Kumar Dwivedi 

机构地区：[1]Division of Pharmaceutics, CSIR-Central Drug Research Institute [2]Division of Medicinal and Process Chemistry, CSIR-Central Drug Research Institute

出　　处：《Journal of Pharmaceutical Analysis》2013年第5期335-340,共6页药物分析学报（英文版）

基　　金：Financial support to Shakti Deep Pachauri and Kiran Khandelwal from the Council of Scientifc and Industrial Research (CSIR)New Delhi;India;is gratefully acknowledged

摘　　要：CDRI compound no. 99/411 is a potent 1,2,4-trioxane antimalarial candidate drug under development at our Institute. An HPLC method for determination of CDRI 99/411 with its starting material and intermediates has been developed and validated for in process quality control and stability studies. The analytical performance parameters such as linearity, precision, accuracy, specificity, limit of detection （LOD） and lower limit of quantification （LLOQ） were determined according to International Conference on Harmonization ICH Q2（R1） guidelines. HPLC separation was achieved on a RP-select B Lichrosphere~ column （250 mm x 4 ram, 5 lam, Merck） using water containing 0.1% glacial acetic acid and acetonitrile as the mobile phase in a gradient elution. The eluents were monitored by a photo diode array detector at 245 and 275 nm. Based on signal to noise ratio of 3 and 10 the LOD of CDRI 99/411 was 0.55 μg/mL, while the LLOQ was 1.05 μg/mL. The calibration curves were linear in the range of 1.05- 68 μg/mL. Precision of the method was determined by inter- and intra-assay variations within the acceptable range.CDRI compound no. 99/411 is a potent 1,2,4-trioxane antimalarial candidate drug under development at our Institute. An HPLC method for determination of CDRI 99/411 with its starting material and intermediates has been developed and validated for in process quality control and stability studies. The analytical performance parameters such as linearity, precision, accuracy, specificity, limit of detection （LOD） and lower limit of quantification （LLOQ） were determined according to International Conference on Harmonization ICH Q2（R1） guidelines. HPLC separation was achieved on a RP-select B Lichrosphere~ column （250 mm x 4 ram, 5 lam, Merck） using water containing 0.1% glacial acetic acid and acetonitrile as the mobile phase in a gradient elution. The eluents were monitored by a photo diode array detector at 245 and 275 nm. Based on signal to noise ratio of 3 and 10 the LOD of CDRI 99/411 was 0.55 μg/mL, while the LLOQ was 1.05 μg/mL. The calibration curves were linear in the range of 1.05- 68 μg/mL. Precision of the method was determined by inter- and intra-assay variations within the acceptable range.

关 键 词：HPLC TRIOXANE Process quality control STABILITY 

分 类 号：R914[医药卫生—药物化学]