Rane V P, Shinde D B
Department of Chemical Technology, Dr. Babasaheb Ambedkar Marathwada University, Aurangabad-431004 (MS), India.
J Chromatogr Sci. 2008 Oct;46(9):772-6. doi: 10.1093/chromsci/46.9.772.
A simple, rapid, and robust liquid chromatography method was developed and validated for the enantiomeric separation of duloxetine in bulk drug substance. The enantiomers of duloxetine were resolved on a Chiralpak AD-H (amylose based stationary phase) column using a mobile phase consisting of n-hexane-ethanol-diethyl amine (80:20:0.2, v/v/v) at a flow rate of 1.0 mL/min. The resolution between the enantiomers was found to be not less than 2.8 in optimized method. The presence of diethyl amine in the mobile phase played an important role in enhancing chromatographic efficiency and resolution between the enantiomers. The developed method was extensively validated and proved to be robust. The calibration curve for (R)-enantiomer showed excellent linearity over the concentration range of 750 ng/mL (LOQ) to 7500 ng/mL. The limit of detection and quantitation for (R)-enantiomer were 250 and 750 ng/mL, respectively. The percentage recovery of the (R)-enantiomer ranged between 98.3% to 101.05% in bulk drug samples of duloxetine. The proposed method was found to be suitable and accurate for quantitative determination of (R)-enantiomer in bulk drug substance.
开发并验证了一种简单、快速且稳健的液相色谱法，用于原料药度洛西汀的对映体分离。度洛西汀的对映体在Chiralpak AD-H（直链淀粉基固定相）柱上分离，流动相由正己烷-乙醇-二乙胺（80:20:0.2，v/v/v）组成，流速为1.0 mL/min。在优化方法中，对映体之间的分离度不低于2.8。流动相中二乙胺的存在对提高色谱效率和对映体之间的分离度起着重要作用。所开发的方法经过广泛验证，证明是稳健的。(R)-对映体的校准曲线在750 ng/mL（定量限）至7500 ng/mL的浓度范围内显示出良好的线性。(R)-对映体的检测限和定量限分别为250和750 ng/mL。度洛西汀原料药样品中(R)-对映体的回收率在98.3%至101.05%之间。所提出的方法被认为适用于原料药中(R)-对映体的定量测定且准确。
