An improved and validated LC method for resolution of bicalutamide enantiomers using amylose tris-(3,5-dimethylphenylcarbamate) as a chiral stationary phase.
An improved and validated LC method for resolution of bicalutamide enantiomers using amylose tris-(3,5-dimethylphenylcarbamate) as a chiral stationary phase.
复制标题
DOI：
10.1016/j.jpba.2006.04.014
复制
发表时间：
2006-09
影响因子：
3.4
通讯作者：
R. Nageswara Rao;A. Narasa Raju;D. Nagaraju
中科院分区：
文献类型：
--
作者：
R. Nageswara Rao;A. Narasa Raju;D. Nagaraju
建立并验证了一种改进的比卡鲁胺对映体纯度测定方法。色谱柱为Chiralpak AD-H(250 mm×4.6 mm；粒径5μm)，流动相为正己烷：异丙醇(65：35 v/v)，流速为1.0ml/m in，检测波长270 nm，检测波长270 nm，旋光检测器串联检测对映体。考察了异丙醇、乙醇和温度对对映体对映体选择性和拆分的影响。方法的准确度、精密度和线性范围为10-250μg/ml，r2为0.9999。对映体的检出限为(2.4，3.0)×10−8g/ml，定量限为(R)-(−)-(2，9)×10-BCT 8g/ml。该方法适用于原料药和制剂中比卡鲁胺对映体纯度的快速测定。
An improved HPLC method for determination of enantiomeric purity of bicalutamide in drugs and pharmaceuticals was developed and validated. Baseline separation with resolution ≥6.0 was achieved within 10min on Chiralpak AD-H (250mm×4.6mm; particle size 5μm) column using n-hexane:2-propanol (65:35 v/v) as mobile phase at a flow rate of 1.0ml/min at 25°C. The detection was made at 270nm using UV detector while a polarimetric detector connected in series was used for identification of enantiomers. The effects of 2-propanol, ethanol and temperature on enantioselectivity and resolution of enantiomers were evaluated. The method was validated in terms of accuracy, precision and linearity in the range of 10–250μg/ml and the r2was >0.9999. The recoveries were 99.68–100.25% with <1% R.S.D. The limits of detection (LOD) and quantification (LOQ) of enantiomers were (2.4, 3.0 and 7.6, 9.3)×10−8g/ml for (S)-(+)-BCT and (R)-(−)-BCT enantiomers, respectively. The method was found to be suitable for rapid determination of enantiomeric purity of bicalutamide in bulk drugs and pharmaceutical formulations.