利用差异衍生同步分析醛糖和酮糖  

Determination of Aldoses and Ketoses by Gas Chromatography/Mass Spectrometry Using Differential Derivatization

作　　者：叶芳挺[1] 严小军[1] 徐继林[1] 陈海敏[1] 

机构地区：[1]宁波大学浙江省海洋生物工程重点实验室,宁波315211

出　　处：《分析化学》2005年第11期1569-1572,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.20472040);国家科技部新药博士基金(No.2003AA2Z3511)资助项目

摘　　要：建立了一种可同时对醛、酮糖进行精确定性和定量分析的方法.以肌醇作为内标,用80%乙醇超声提取,利用醋酸酐和HMDS+TMCS(1∶ 3)进行差异衍生,在EI源下用SIM模式进行GC/MS分析.结果表明:11种标准单糖在1～4 mg/L范围内线性良好;仪器检出限:醛糖在8.15～22.4 μg/L之间;酮糖为2.32 μg/L和3.47 μg/L;高、中、低3个量的平均回收率在73.0%～95.7%,相对标准偏差在3.1%～10.0%.对枸杞游离单糖进行测定,各单糖含量分别在0.26～368.6 mg/g.该方法弥补了以前单糖分析中的缺陷,对既含有醛糖又含有酮糖的样品可同时进行精确的定性定量分析.To establish a new method to determine aldoses and ketoses simultaneously, the monosaccharides were extracted with 80% ethanol after sonication for 15 min and this process was repeated three times. The extract was evaporated under vacuum. Suger oximes were formed using hydroxylamine and pyridine under heating at 90℃ for 30 min. After reaction, the sample was divided into two parts. One part was added by pyridine and acetic anhydride for derivatization at 90℃ for 30 min, the other part was added by hexamethyldisiazane （HMDS） and trimethylchlorosilane （TMCS） for silylation reaction at 80℃ for 1 h. The two parts were analyzed by gas chromatography/mass spectrometry （GC-MS） in selected ion monitoring （SIM） mode, and inositol was used as internal standard. Results indicate that the linearity is superior in 1 - 4 mg/L, the detection limit of aldoses is 8.15 - 22.39 μg/L, whereas ketoses from 2.32 μg/L to 3.47 μg/L. The average recovery rate is from 73.0 % to 95.7% and the RSDs were 3.1% - 10.0%. The free monosaccharides in Lyceum barbarum L. was determined by this method with the results of 0.26 - 368.6 mg/g.

关 键 词：差异衍生 醛糖 酮糖 色谱/质谱 同步分析 利用差异 衍生 相对标准偏差 定性定量分析 GC/MS分析 

分 类 号：O656[理学—分析化学]