【摘要】 采用反相高效液相色谱(RP-HPLC)与质谱(MS)联用技术对固相法化学合成七肽(H2N-PFNSLAI-COOH,M r 760.9)时出现的消旋产物进行了分析。根据弱疏水性合成七肽粗品特性,提出了充分利用吸附和分配双重保留机制的“早期吸附”概念,以此优化色谱条件得到4个峰形良好的色谱峰;质谱分析表明:4谱峰具有相同的m/z761.5[M+H]+值,对每一消旋产物进行在线多肽测序,并利用串联质谱(MSn)谱图叠加的方法,得到b轴和y轴两套片段信息,成功确定了合成七肽的4个消旋产物。更多还原

【Abstract】 Reversed phase high performance liquid chromatograghy（RP-HPLC）/mass spectrometry（MS） was used for the determination of racemization products of solid-phase chemically synthesized heptapepetide(H₂N-PFNSLAI-COOH,Mr 760.9).Based on the physicochemical property of weak hydrophobic heptapeptide,the concept of pre-adsorption′ was proposed in order to take full advantage of partition and adsorption retention mechanisms for separation.Using this method,four ideal RP-HPLC peaks were obtained by optimizing chromatographic conditions.Meanwhile,the MS information indicated that four peaks had the same value of m/z 761.5[M-H]⁺.Through simultaneous peptide sequencing of each racemization product and spectrum superposition of different tandem MS(MSⁿ),the two sets of fragment ions,b and y,were observed,which demonstrated that four racemization products of synthetic heptapeptide were successfully identified.更多还原