Development and validation of an HPLC method for the determination of process-related impurities in pridinol mesylate, employing experimental designs
Development and validation of an HPLC method for the determination of process-related impurities in pridinol mesylate, employing experimental designs
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DOI：
10.1016/j.aca.2009.09.022
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发表时间：
2009-11-10
影响因子：
6.2
通讯作者：
Kaufman, Teodoro S.
中科院分区：
文献类型：
--
作者：
Bianchini, Romina M.;Castellano, Patricia M.;Kaufman, Teodoro S.
高效液相色谱法测定中枢抗胆碱能化合物甲磺酸吡啶地诺原料药中的工艺杂质。已经开发和验证。使用光谱表征的合成杂质作为标准品。采用实验设计策略优化色谱分离，并在C-18柱上实现色谱分离，其中移动的流动相含有50 mM磷酸钾缓冲液（pH 6.4），MeOH和2-丙醇（20：69：11，v/v/v），流速为1.0 mL min（-1）。在245 nm处进行UV检测。当用二极管阵列检测器记录色谱图并评价峰纯度（>0.9995）时，彻底验证了优化方法，证明具有选择性。该方法在0.05-2.5%（相对于两种工艺相关杂质的1%质量标准限度为5-250%）范围内具有耐用性和线性（r（2）> 0.99）;在重复性（RSD）方面也具有精密度
A simple high performance liquid chromatographic method for the determination of process-related impurities in bulk drug of the central anticholinergic compound pridinol mesylate. has been developed and validated. Spectroscopically characterized synthetic impurities were used as standards. The chromatographic separation was optimized employing an experimental design strategy, and was achieved on a C-18 column with a mobile phase containing 50 mM potassium phosphate buffer (pH 6.4), MeOH and 2-propanol (20:69:11, v/v/v), delivered at a flow rate of 1.0 mL min(-1). UV detection was performed at 245 nm. The optimized method was thoroughly validated, demonstrating to be selective, when the chromatogram was recorded with a diode-array detector and peak purities were evaluated (>0.9995). The method is robust and linear (r(2) > 0.99) over the range 0.05-2.5% (5-250% with regards to the 1% specification limit for both process-related impurities); it is also precise, regarding repeatability (RSD