GITC柱前衍生化RP-HPLC检测吡喹酮中间体的对映异构体  

Enantiomers Detection of Praziquantel Intermediates by RP-HPLC after GITC Pre-Column Derivatization

作　　者：郑小红[1] 邵强 蒋红艳[1] 

机构地区：[1]重庆医药高等专科学校药学院,重庆400030 [2]东芝医疗系统(中国)有限公司,北京100015

出　　处：《世界科技研究与发展》2016年第3期626-629,641,共5页World Sci-Tech R&D

基　　金：国家自然科学基金(30772595;30171070);科技部重大专项(2010ZX09401-306-1-1);重庆市卫生和计划生育委员会项目(20142120);重庆医药高等专科学校校级重点项目(ygz2014103)资助

摘　　要：目的建立柱前衍生化反相高效液相色谱法（RP-HPLC）,分离和检测吡喹酮中间体1-[（苯甲酰氨基）甲基]-1,2,3,4-四氢异喹啉（BTIQ）的对映异构体。方法以2,3,4,6-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯（GITC）作柱前衍生化试剂,考察衍生化试剂用量、反应溶剂、衍生化时间、流动相组成、柱温等因素对手性BTIQ分离和检测的影响。结果衍生化产物在C18柱（250 mm×4.6 mm,5μm）上进行分离,较优色谱分离条件为以乙腈-0.02 mol/LKH2PO4（40∶60,v/v）为流动相,检测波长为250 nm,流速1.5 ml/min,柱温30℃。在该色谱条件下BTIQ衍生物可达到基线分离,分离度为2.1,非对映异构体的保留时间在40 min以内。在2~320μg/ml范围内BTIQ对映异构体浓度和峰面积线性关系良好。结论本文所建立的方法简便、快速、可靠,可用于吡喹酮中间体BTIQ的手性分离,也可为其光学纯度的质量控制提供参考。Objective To establish a method for separation of the enantiomers of praziquantel intermediates1-（ Benzamidomethyl）-1,2,3,4-tetrahydro-isoquinoline（ BTIQ） based on reversed phase high performace liquid chromatography（ RPHPLC） after the pre-column derivatization.Methods The separation of BTIQ enantiomer was studied using 2,3,4,6-tetraO-acetyl-（ β-D-glycosyl）-isothiocyanate（ GITC） as the pre-column chiral derivatizing reagent.The effects of reaction solvent,the derivation time,the mount of GITC and the chromatography conditions such as the composition of the mobile phase,the column temperature were investigated.Results A baseline separation of BTIQ was achieved within 40 minutes in a C18 column（250 mm×4.6 mm,5 μm） with a binary solvent mixture of acetonitrile and 0.02 mol/L potassium dihydrogen phosphate（ 40∶ 60,v/v） as the optimized chromatographic conditions.The flow rate was 1.5 ml/min,the UV detector was set at 250 nm and the column temperature was set at 30℃.A good linear correlation was observed between the peak area and the concentration within 2~320 μg/ml.Conclusion The method mentioned above is feasible,rapid and could be used for the separation and quality control of the enantiomers of BTIQ.

关 键 词：反相高效液相 GITC 柱前衍生化 吡喹酮中间体 对映体 

分 类 号：TQ460.1[化学工程—制药化工]