新型糖组成高效液相色谱分析技术的构建及其在水飞蓟多糖质控中的应用  

Development of a new HPLC technique for analyzing monosaccharide composition and its application in the quality control of Silybum marianum polysaccharide

作　　者：田灵敏[1] 邱雪梅[1] 潘子敬[1] 吕游[1] 杨兴斌[1] 

机构地区：[1]陕西师范大学生命科学学院,教育部药用植物资源与天然药物化学重点实验室,陕西西安710062

出　　处：《药学学报》2010年第4期498-504,共7页Acta Pharmaceutica Sinica

基　　金：国家自然科学基金资助项目(C30972054);陕西省自然科学基金资助项目(2007C223)

摘　　要：本研究采用1-苯基-3-甲基-5-吡唑啉酮(PMP)作为还原醛糖的标记识别分子,利用高效液相色谱-紫外检测器(HPLC-UV)和普通C18色谱柱,建立了10种常见单糖在13.5min内的快速HPLC-UV分析鉴别技术,并成功地用于植物药水飞蓟多糖中单糖的组成分析。结果表明,醛糖的PMP标记与流动相三乙胺(TEA)配比分离调节相结合,可大幅度调节系列单糖PMP标记物的分离度,具有很高的分离可控性;水飞蓟多糖由甘露糖、鼠李糖、葡萄糖醛酸、半乳糖醛酸、葡萄糖、木糖、半乳糖及阿拉伯糖8种单糖组成,其摩尔比为0.66∶0.84∶0.58∶1.0∶1.6∶0.69∶2.7∶4.8;样品测定回收率为92.4%～104.0%。该方法简单、快速、准确,可用于水飞蓟多糖的有效质量控制。A new HPLC-UV technique for the separation and analysis of 10 monosaccharides achieved within 13.5 min using 1-phenyl-3-methyl-5-pyrazolone （PMP） as the labelling molecule of the reductive monosaccharides has been established by combining common high performance liquid chromatography-UV and C18 column. The established technique was applied to the quantification of the monosaccharide components in extract of Silybum marianum. The results showed that the tested 10 monosaccharides as PMP derivatives were baseline separated under the HPLC conditions proposed. It was confirmed that Silybum marianum extract was composed of mannose,rhamnose,glucuronic acid,galacturonic acid,glucose,xylose,galactose and arabinose with the molar ratio of 0.66∶0.84∶0.58∶1.0∶1.6∶0.69∶2.7∶4.8. Quantitative recoveries of the compositional monosaccharides separated from the extract were in the range of 92.4% -104.0%,and the RSD values fell within 0.68% -3.81%. The results demonstrated that the proposed HPLC method was simple,rapid,convenient,and precise,and it was applicable to the analysis of the compositional monosaccharides of Silybum marianum extract.

关 键 词：水飞蓟多糖 质量控制 单糖组成 RP-HPLC 

分 类 号：R917[医药卫生—药物分析学]