Abstract

A simple, sensitive and accurate reversed-phase high-performance liquid chromatography (RP-HPLC) method was established for the determination of piperidine and piperidine hydrochloride in artane, using pre-column derivatization with 4-toluenesulfonyl chloride. The RP-HPLC method was carried out on a Inertsil C18 column (250 × 4.6 mm I.D.) maintained at 30°C. The mobile phase consisted of water with 0.1% phosphoric acid (phase A) and acetonitrile (phase B) (32:68, V:V) at a flow rate of 1.0 mL/min. Linearity of piperidine was found in the range of 0.44–53.33 μg/mL with R² = 0.9996. The limit of detection was estimated to be 0.15 μg/mL, and the limit of quantitation was 0.44 μg/mL. The average recovery was 101.82% with relative standard deviations of 0.6% at three spiked levels. The developed method using HPLC-ultraviolet system was a rapid tool for routine analysis of piperidine in the bulk form with good accuracy.

中文翻译：

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使用 4-甲苯磺酰氯进行柱前衍生的 RP-HPLC 分析阿坦中哌啶的总含量

摘要

建立了一种简单、灵敏、准确的反相高效液相色谱 (RP-HPLC) 方法，采用 4-甲苯磺酰氯进行柱前衍生化测定阿坦中哌啶和哌啶盐酸盐的含量。RP-HPLC 方法在保持在 30°C 的 Inertsil C18 柱（250 × 4.6 mm ID）上进行。流动相由具有 0.1% 磷酸的水（A 相）和乙腈（B 相）（32:68，V:V）组成，流速为 1.0 mL/min。哌啶的线性范围为 0.44–53.33 μg/mL，R ² = 0.9996。检测限估计为 0.15 μg/mL，定量限为 0.44 μg/mL。三个加标水平的平均回收率为 101.82%，相对标准偏差为 0.6%。所开发的使用 HPLC-紫外系统的方法是常规分析散装哌啶的快速工具，具有良好的准确性。