反相离子对液相色谱测定葡萄糖化学氧化过程中的6种有机酸  

Determination of six organic acids in chemical oxidation process of glucose by ion-pair reversed phase HPLC

作　　者：朱璇[1] 余作龙[1] 周佳栋[1] 姚琴[1] 曹飞[1] 韦萍[1] 

机构地区：[1]南京工业大学生物与制药工程学院,南京210009

出　　处：《分析试验室》2013年第5期20-24,共5页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金项目(21106063;30900009);江苏省自然科学基金项目(BK2010557)资助

摘　　要：建立了反相离子对液相色谱同时测定葡萄糖氧化产物:葡萄糖醛酸、葡萄糖酸、乙醇酸、乙酸、葡萄糖二酸及酒石酸含量的方法。采用kromasil C18色谱柱(250 mm×4.6 mm,5μm),流动相为10 mmol/L K2HPO4-10 mmol/L四丁基硫酸氢铵(pH 7.2):甲醇(95:5,V/V),检测波长210 nm,流速0.7 mL/min,进样量20μL。6种有机酸在线性范围内峰面积与浓度呈良好的线性关系;回收率为92.7%～107.0%;RSD(n=5)为0.9%～6.3%。20 min内即可将6种物质分开。对葡萄糖化学氧化过程检测表明,HNO3氧化法反应剧烈,除了生成葡萄糖酸、葡萄糖醛酸和葡萄糖二酸外,还生成碳-碳键断裂的副产物如酒石酸、乙醇酸等,而TEMPO法反应较为温和,并未发生碳-碳键断裂。Glucose oxidation products including glucuronic acid, gluconic acid, glycolic acid, acetic acid, glucaric acid, tartaric acid were detected simultaneously by an ion-pair reversed phase chromatography. The optimum analytical conditions were： 10 mmol/L K2HPO4 - 10 mmol/L tetrabutylammonium hydrogen sulfate （adjusted to pH 7.2 with KOH solution） ： methanol （95：5, V/V） as mobile phase, kromasil C18as column, k = 210 nm and 0. 7 mL/min as flow rate. Six compounds were separated completely and eluted in 20 rain. The average recoveries were in the ranged of 92. 7% - 107.0% , and the relative standard deviations were in the range of 0. 9% ~6.3% （n =5）. The chemical oxidation processes of glucose were detected by this method. In HNO3 oxidation reaction, the reaction was acute and the carbon-carbon broken bond by-products such as tartaric acid ,glycolic acid ,acetic acid were detected. On the contrast, the reaction was moderate by TEMPO method and the only three compounds of glucuronic acid,gluconic acid and glucaric acid were detected.

关 键 词：离子对液相色谱 葡萄糖氧化 有机酸 葡萄糖二酸 

分 类 号：O657.7[理学—分析化学]