色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
12期
1306-1312
,共7页
梁图%傅青%辛华夏%李芳冰%金郁%梁鑫淼
樑圖%傅青%辛華夏%李芳冰%金鬱%樑鑫淼
량도%부청%신화하%리방빙%금욱%량흠묘
部分酸水解%亲水作用色谱%质谱%多糖%黄芪%表征
部分痠水解%親水作用色譜%質譜%多糖%黃芪%錶徵
부분산수해%친수작용색보%질보%다당%황기%표정
partial acid hydrolysis%hydrophilic interaction liquid chromatography(HILIC)%mass spectrometry(MS)%polysaccharides%Astragalus%characterization
来自中药的水溶性多糖具有广谱治疗和低毒性特点,是天然药物及保健品研发中的重要组成部分。针对中药多糖结构复杂、难以表征的问题,本文以中药黄芪中的多糖为研究对象,采用“自下而上”法完成对黄芪多糖的表征。首先使用部分酸水解方法水解黄芪多糖,分别考察了水解时间、酸浓度和温度的影响。在适宜条件(4 h、1.5 mol/L三氟乙酸、80℃)下,黄芪多糖被水解为特征性的寡糖片段。接下来,采用亲水作用色谱与质谱联用对黄芪多糖部分酸水解产物进行分离和结构表征。结果表明,提取得到的黄芪多糖主要为1→4连接线性葡聚糖,水解得到聚合度4~11的葡寡糖。本研究对其他中药多糖的表征具有一定的示范作用。
來自中藥的水溶性多糖具有廣譜治療和低毒性特點,是天然藥物及保健品研髮中的重要組成部分。針對中藥多糖結構複雜、難以錶徵的問題,本文以中藥黃芪中的多糖為研究對象,採用“自下而上”法完成對黃芪多糖的錶徵。首先使用部分痠水解方法水解黃芪多糖,分彆攷察瞭水解時間、痠濃度和溫度的影響。在適宜條件(4 h、1.5 mol/L三氟乙痠、80℃)下,黃芪多糖被水解為特徵性的寡糖片段。接下來,採用親水作用色譜與質譜聯用對黃芪多糖部分痠水解產物進行分離和結構錶徵。結果錶明,提取得到的黃芪多糖主要為1→4連接線性葡聚糖,水解得到聚閤度4~11的葡寡糖。本研究對其他中藥多糖的錶徵具有一定的示範作用。
래자중약적수용성다당구유엄보치료화저독성특점,시천연약물급보건품연발중적중요조성부분。침대중약다당결구복잡、난이표정적문제,본문이중약황기중적다당위연구대상,채용“자하이상”법완성대황기다당적표정。수선사용부분산수해방법수해황기다당,분별고찰료수해시간、산농도화온도적영향。재괄의조건(4 h、1.5 mol/L삼불을산、80℃)하,황기다당피수해위특정성적과당편단。접하래,채용친수작용색보여질보련용대황기다당부분산수해산물진행분리화결구표정。결과표명,제취득도적황기다당주요위1→4련접선성포취당,수해득도취합도4~11적포과당。본연구대기타중약다당적표정구유일정적시범작용。
Water-soluble polysaccharides from traditional Chinese medicine(TCM)have prop-erties of broad-spectrum treatment and low toxicity,making them as important components in natural medicines and health products. In order to solve the problem of polysaccharides charac-terization caused by their complex structures,a“bottom-up”approach was developed to com-plete the characterization of polysaccharides from Astragalus. Firstly,Astragalus pieces were extracted with hot water and then were precipitated by ethanol to obtain Astragalus polysaccha-rides. Secondly,a partial acid hydrolysis method was carried out and the effects of time,acid concentration and temperature on hydrolysis were investigated. The degree of hydrolysis increased along with the increase of hydrolysis time and acid concentration. The temperature played a great role in the hydrolysis process. No hydrolysis of the polysaccharides occurred at low temperature,while the polysaccharides were almost hydrolyzed to monosaccharide at high temperature. Under the optimum hydrolysis conditions(4 h,1. 5 mol/L trifluoroacetic acid, and 80 ℃),Astragalus polysaccharides were hydrolyzed to characteristic oligosaccharide frag-ments. At last,a hydrophilic liquid chromatography-mass spectrometry method was used for the separation and structural characterization of the polysaccharide hydrolysates. The results showed that the resulting polysaccharides were mainly 1→4 linear glucan,and gluco-oligosac-charides with the degrees of polymerization(DP ) of 4-11 were obtained after partial acid hydrolysis. The significance of this study is that it is the guidance for the characterization of other TCM polysaccharides.