L-羟脯氨酸寡肽混合物的高效液相色谱分离与质谱分析  

Isolation and Identification of the Mixture of L-Hydroxyproline Oligo-Peptides by Reversed-Phase High Performance Liquid Chromatography and Electrospray Ionization Tandem Mass Spectrometry

作　　者：孙艳亭[1] 卢奎[1] 马丽[1] 曹书霞[2] 赵玉芬[2] 

机构地区：[1]河南工业大学化学化工学院,河南郑州450052 [2]郑州大学化学系化学生物学重点实验室,河南郑州450052

出　　处：《色谱》2007年第4期524-527,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金资助项目(Nos.20272055;20572016);河南省杰出青年科学基金资助项目(No.0312000900);河南省教育厅科技计划资助项目(2006KYCX017;200510459015)

摘　　要：研究了三氯氧磷辅助下L-羟脯氨酸的成肽反应,建立了采用反相高效液相色谱-质谱/质谱联用技术分离鉴定羟脯氨酸寡肽混合物的方法,优化了L-羟脯氨酸寡肽混合物的色谱分离条件。实验以YWG C8柱(10μm,250mm×10mm)为分离柱,以乙腈-0.06%三氟乙酸水溶液(体积比为2∶98)为流动相进行等度洗脱,在正离子模式下对洗脱物进行了电喷雾电离串联质谱鉴定。结果显示,分离出的各组分分别为L-羟脯氨酸二肽、L-羟脯氨酸环二肽和L-羟脯氨酸三肽。A reversed-phase high performance liquid chromatographic-electrospray ionization tandem mass spectrometric method （ RP-HPLC/MS^2 ） was developed for the analysis and identi-fication of a reaction mixture of L-hydroxyproline oligo-peptides. The mixture was separated on a YWG C8 column （ 10 μm, 250 mm × 10 mm） using acetonitrile-watr containing 0.06% trifluoroacetic acid （2： 98, v/v） as the mobile phase. The separation conditions were optimized. The mixture was analysed with electrospray ionization mass spectrometry （ESI-MS） and ESI- MS/MS in positive mode. MS and MS2 spectra of individual chromatographic peak were ob-tained. It indicated that there were hydroxyproline dipeptide, hydroxyproline tripeptide and hydroxyproline cyclo-dipeptide in the mixtures, besides hydroxyproline. The described method can be effectively applied to perform identification of hydroxyproline oligo-peptide mixtures.

关 键 词：反相高效液相色谱 电喷雾串联质谱 L-羟脯氨酸寡肽混合物 

分 类 号：O658[理学—分析化学]