反相高效液相色谱/电喷雾质谱法分析化学合成七肽粗产物  

Analysis of Crude Synthetic Product of a Heptapeptide by Reversed Phase High Performance Liquid Chromatography/ Electrospray-Mass Spectrometry

作　　者：王贤纯[1] 梁宋平[1] 

机构地区：[1]湖南师范大学生命科学学院,长沙410081

出　　处：《分析化学》2004年第9期1219-1222,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金 (No .3 9990 60 0 );湖南省自然科学基金 (No .0 1JJY2 0 2 8)资助项目

摘　　要：利用RP HPLC/ESI MS直接分析用芴甲氧羰基 (Fmoc)固相多肽合成方法在PHB树脂上偶联合成的一个七肽 (H2 N Tyr Val Asn Thr Asn Met Gly CO0H ,Mr 797.3 )粗产物。RP HPLC显示合成粗产物含有 1个主成分 ,4个次要成分和多个微量成分 ;与之联用的电喷雾质谱则同步准确地测定出各成分的分子量 (m/z)并自动对各主要成分的化学结构进行了串联质谱分析。结果证明 ,粗产物中的主成分即为目标七肽 ,另外几个主要副产物为七肽的氧化产物或残缺肽。In order to investigate the application of reversed-phase high performance liquid chromatography (RP-HPLC)/ion trap electrospray mass spectrometry (ESI-MS) to the solid-phase chemically synthesized peptides and the mechanism of side reactions, RP-HPLC/ESI-MS was applied to the direct analysis of a crude product of heptapeptide (H2N-Tyr-Val-Asn-Thr-Asn-Met-Gly-COOH, Mr 797.3) solid-phase chemically synthesized in stepwise fashion using Fmoc chemistry on a PHB resin manually. RP-HPLC showed that the crude product contained one major component, four minor components and several trace-level components. The accurate molecular weight of each component was determined by the coupled electrospray mass spectrometry and the structural analysis of the main components was done by tandem mass spectrometry (MS/MS) synchronously. The results show that the major component of the crude product is the desired heptapeptide and the main by-products are derived from the oxidation or deformity of the desired peptide.

关 键 词：七肽 粗产物 反相高效液相色谱 电喷雾质谱法 固相化学合成 

分 类 号：O657.63[理学—分析化学]