Hunan Key Lab of Biomedical Materials and Devices, College of Life Sciences and Chemistry, Hunan University of Technology, Zhuzhou 412008, China.
State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Changsha 410082, China.
J Chromatogr Sci. 2022 Sep 3;60(7):613-619. doi: 10.1093/chromsci/bmab099.
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.
建立了一种简单、灵敏、准确的反相高效液相色谱（RP-HPLC）法，用于测定安坦中哌啶和盐酸哌啶，采用 4-甲苯磺酰氯柱前衍生化。RP-HPLC 法在 Inertsil C18 柱（250×4.6mm ID）上进行，在 30°C 下保持。流动相由水（含 0.1%磷酸）和乙腈（32:68，V:V）组成，流速为 1.0mL/min。哌啶在 0.44-53.33μg/mL 范围内呈线性，R2=0.9996。检测限估计为 0.15μg/mL，定量限为 0.44μg/mL。在三个加标水平下，平均回收率为 101.82%，相对标准偏差为 0.6%。该 HPLC-紫外系统建立的方法是一种快速工具，可用于常规分析原料药中的哌啶，具有良好的准确性。
