N-乙酰-D-葡萄糖胺差向异构体及有关物质的HPLC研究  

Studies on the epimers and the related substances of N-Acetyl-D-Glucosamine by HPLC

作　　者：侯卫南[1] 王健[1] 聂晓明[1] 杨腊虎[2] 

机构地区：[1]江苏江山制药有限公司,江苏靖江214500 [2]中国药品生物制品检定所,北京100050

出　　处：《药物分析杂志》2008年第7期1117-1120,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:对 N-乙酰-D-葡萄糖胺差向异构体和有关物质进行研究。方法:建立高效液相色谱法分离异构体及有关物质。色谱柱:Alltima C_(18)(250 mm×4.6 mm,5 μm),流动相:水,流速:0.8 mL·min^(-1),检测波长:193 nm,进样:20 μL。HPLC/MS 研究有关物质归属,APCI 正离子模式。半制备-HPLC 法提取有关物质,色谱柱:Zorbax SB C_(18)(9.6 mm×250 mm,10μm),流动相:水,流速:3 mL·min^(-1),样品浓度:80 mg·mL^(-1),进样:100 μl。结果:N-乙酰-D-葡萄糖胺溶于水后自α型差向异构体向β型转化并最终达到平衡,初步研究表明本品固态为α构型;样品中有关物质为二乙酰基葡萄糖胺,水溶液中同样存在可互相转化的差向异构体。结论:用 HPLC 法可定量测定样品水溶液中平衡时α、β构型比例,并可检测样品有关物质的含量,为制定质量标准提供可靠依据。Objective： Studies on the anomeric conversion of α - epimer toβ- epimer in water and the related substances of N - Acetyl - D - Glucosamine. Methods ： An optioned HPLC has been developed for seperation of the epimers and the related substances,coloum： Alhima C18 （250 mm × 4.6 mm,5 μm） ,mobile phase： water,flow rate： 0. 8 mL · min^-1, detector wavelength： 193nm. The related substances were identified by HPLC/MS,APCI in positive ion mode. Semi - Prep HPLC is used to extract the related substances, coloum：Zorbax SB C18 （250 mm × 9.6 mm, 10 μm） , mobile phase ： water, flow rate ： 3 mL · min ^- 1, sample concentration ： 80 mg · mL^- 1, injection volume： 100 μl. Results ：N- Acetyl- D- Glucosamine has a process of anomeric conversion from the α- epimer toβ - epimer in water and the balance of α,β - anomeric conversion was made. The related substances were indentified as two convertiable epimers of Diacetyl Glucosamine. Conclusion：The HPLC method could work out the content of the epimers α-andβin water solution in equilibrium, also it is suitable for the determation of the related substances of N - Acetyl - D - Glucosamine.

关 键 词：N-乙酰-D-葡萄糖胺 高效液相色谱法 差向异构体 有关物质 二乙酰基葡萄糖胺 

分 类 号：R978.15[医药卫生—药品] R284.1[医药卫生—药学]