快速柱前衍生HPLC法检测曲格列汀中(R)-3-氨基哌啶  

Determination of (R)-3-aminopiperidine in trelagliptin by fast pre-column derivatization and HPLC

作　　者：曲喜龙 李铁健 刘治军 张贵民 QU Xilong;LI Tiejian;LIU Zhijun;ZHANG Guimin(Shandong New Time Pharmaceutical Co.,Ltd.,National Chiral Pharmaceutical Engineering and Technology Research Center,Linyi 273400)

机构地区：[1]山东新时代药业有限公司,国家手性制药工程技术研究中心,临沂273400

出　　处：《分析试验室》2021年第3期361-365,共5页Chinese Journal of Analysis Laboratory

摘　　要：以邻苯二甲醛(OPA)和3-巯基丙酸为衍生试剂,建立了柱前衍生高效液相色谱(HPLC)测定曲格列汀中(R)-3-氨基哌啶含量的分析方法。(R)-3-氨基哌啶与衍生剂在碱性(p H 10.5)条件下于室温反应30s,进行柱前衍生,并利用高效液相色谱-质谱对衍生产物进行定性分析。采用YMC-Triart C18色谱柱(150 mm×4.6 mm,5μm)分离,流动相采用0.05 mol/L乙酸钠(p H 6.0)-甲醇溶液,梯度洗脱,流速1.0 mL/min,检测波长331 nm,柱温30℃。(R)-3-氨基哌啶质量浓度在0.08~2.0μg/mL范围内线性关系良好(r=0.9993),定量限为1.6 ng,加标回收率在98.0%~10^(6).9%之间,相对标准偏差(RSD)为2.8%。该方法可用于曲格列汀中(R)-3-氨基哌啶含量测定。An analytical method was developed for the determination of(R)-3-aminopiperidine in trelagliptin by high performance liquid chromatography(HPLC) coupled with pre-column derivatization using ophthalaldehyde(OPA) and 3-mercaptopropionic acid as the derivatization reagent.(R)-3-aminopiperidine reacted with derivatization reagent in the alkaline environment(p H 10.5) under room temperature for 30 s.The derivatization products were identified by HPLC-mass spectrometry(MS).The separation was carried out on YMC Triart C18 column(150 mm × 4.6 mm,5 μm) by using a gradient elution system of methanol-0.05 mol/L sodium acetate solution(pH 6.0) at a flow rate of 1.0 m L/min,detection wavelength at 331 nm,and column temperature at 30℃ . The calibration curve for(R)-3-aminopiperidine revealed good linearity in the range of0.08-2.0 μg/m L(r = 0.9993).The limit of quantitation was 1.6 ng and the recoveries of the spiked samples were 98.0%-10^(6).9%.The relative standard deviation was 2.8%.The method is suitable for the determination of(R)-3-aminopiperidine in trelagliptin.

关 键 词：高效液相色谱 柱前衍生 (R)-3-氨基哌啶 邻苯二甲醛 3-巯基丙酸 

分 类 号：R917[医药卫生—药物分析学]