摘要
目的建立泡核桃壳多糖中单糖的组成和定量的检测方法。方法以三氟乙酸水解核桃壳多糖,所获得的多糖水解物加入衍生化试剂1-苯基-3-甲基-5-吡唑酮(PMP)柱前衍生化,利用高效液相色谱法分析单糖的PMP衍生物。Agilent Venusil XBP-C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-醋酸铵缓冲液(pH 5.5)19∶81,体积流量为1.0 mL/min,检测波长为250 nm,柱温为30℃。结果泡核桃壳多糖由D-甘露糖、鼠李糖、半乳糖、D-半乳糖醛酸、葡萄糖、D-葡萄糖醛酸、D-阿拉伯糖等11种单糖(有4种未鉴定出的单糖)组成。D-甘露糖、鼠李糖、D-葡萄糖醛酸、D-半乳糖醛酸、D-葡萄糖、D-半乳糖、D-阿拉伯糖的线性分别为0.041 8～2.09μg,0.045 9～2.295μg,0.043 5～2.175μg,0.042 7～2.135μg,0.040 5～2.026μg,0.043 9～2.195μg,0.047 5～2.375μg;平均加样回收率分别为95.9%、103.1%、104.6%、97.5%、95.8%、87.5%、98.1%,RSD均小于3.0%。在泡核桃壳提取物中D-阿拉伯糖的相对平均含有量最高。结论该方法可以准确地测定出泡核桃壳多糖中含有的单糖及其含有量。
AIM To establish the determination method for analysing monosaccharide composition of polysaccharide from Juglans sigillata.METHODS The walnut shell polysaccharide was hydrolyzed by trifluoroacetic acid to give the hydrolysate containing monosaccharide which reacted with PMP to produce the PMP derivatives.The PMP derivatives were analyzed by HPLC.The concentration of gentiopicroside determined by RP-HPLC method was carried out on Agilent Venusil XBP-C18 column（4.6 mm×250 mm,5 μm）,and the mobile phase was composed of acetonitrile-ammonium acetate buffer（pH 5.5）（19∶ 81）.The flow rate was 1.0 mL/min,and the detection wavelength was set at 250 nm with column temperature of 30 ℃.RESULTS The polysaccharide from Juglans sigillata was broken into mannose,rhamnose,galactose,D-（＋） galacturonic acid,glucose,D-glucuronic acid and D（-） arabinose（included four unidentifiable monosaccharide） with the linear ranges of 0.041 8-2.09 μg,0.045 9-2.295 μg,0.043 5-2.175 μg,0.042 7-2.135 μg,0.040 5-2.026 μg,0.043 9-2.195 μg and 0.047 5-2.375 μg,respectively,and with the average recoveries of 95.9%,103.1%,104.6%,97.5%,95.8%,87.5%,98.1%,respectively.The RSD,were less than 3.0%.The average content of highest among walnut shell extracts was D（-） arabinose.CONCLUSION This method can accurately determine the monosaccharide compositions and contents of polysaccharide from Juglans sigillata.
出处
《中成药》
CAS
CSCD
北大核心
2012年第12期2372-2376,共5页
Chinese Traditional Patent Medicine
关键词
高效液相色谱法
核桃壳多糖
单糖组成
衍生化
HPLC
walnut shell polysaccharide
monosaccharide composition
derivatization
