色谱2012，Vol.30Issue(4)：395-399,5.DOI:10.3724/SP.J.1123.2011.12061
高效离子交换色谱-电化学检测法测定药物合成中间体中的6-磷酸甘露糖
Determination of mannose-6-phosphate in pharmaceutical intermediates by high performance ion-exchange chromatography-electrochemical detection
摘要
Abstract
A novel method was developed for the determination of mannose-6-phosphate and the phosphate in pharmaceutical intermediates by high performance ion-exchange chromatogra-phy (IC) and electrochemical detection. The sample was dissolved with purified water, filtrated by a 0. 22 p.m nylon filter membrane, and then separated by ion-exchange chromatography. The separation was performed on an lonPac AS18 column (250 mm×4 mm) with an IonPac AG18 (SO mm×4 mm) as guard column, and 25 mmol/L KOII solution as the eluent at a flow rate of 1.0 mL/min. The detection was performed with electrochemical detectors (an integrated pulsed amperometric detector and a suppressed conductivity detector in line). Mannose-6-phosphate was selectively determined with an integrated pulsed amperometric detector first. Then, both of mannose-6-phosphate and phosphate were determined with a suppressed conductivity detector after the background conductance of KOH was suppressed with the ASKS suppressor. The injection volume was 25 p,L. The external standard calibration curve was used for quantitative analysis. With an amperometric detector, the linear range of the method for man-nose -6-phosphate were 0.06 - 10.0 mg/L (r =0.999 8). The recoveries were 92. 1% -103. 1% with the relative standard deviations (RSDs) less than 3%. The detection limit was 0. 02 mg/L for mannose-6-phosphate. The method is simple, effective, sensitive and selective. It can be used to determine the quality of pharmaceutical intermediates.关键词
离子交换色谱/安培检测器/电导检测器/串联检测/6-磷酸甘露糖/药物合成中间体Key words
ion-exchange chromatography (IEC)/amperometric detector/conductivity detector/ tandem detection/ mannose-6-phosphate (M6P)/ pharmaceutical intermediates分类
化学化工引用本文复制引用
潘广文,刘绿叶,叶明立,胡忠阳..高效离子交换色谱-电化学检测法测定药物合成中间体中的6-磷酸甘露糖[J].色谱,2012,30(4):395-399,5.基金项目
安徽省教育厅高校省级科学研究项目(KJ2011B211). （KJ2011B211）
