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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

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【作者】 孙艳亭卢奎马丽曹书霞赵玉芬

【Author】 SUN Yanting1,LU Kui1,MA Li1,CAO Shuxia2,ZHAO Yufen2,3(1.School of Chemistry and Chemical Engineering,Henan University of Technology,Zhengzhou 450052,China;2.Key Laboratory for Chemical Biology,Department of Chemistry,Zhengzhou University,Zhengzhou 450052,China;3.Department of Chemistry,Xiamen University,Xiamen 361005,China)

【机构】 河南工业大学化学化工学院郑州大学化学系化学生物学重点实验室郑州大学化学系化学生物学重点实验室 河南郑州450052河南郑州450052厦门大学化学系福建厦门361005

【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。

【Abstract】 A reversed-phase high performance liquid chromatographic-electrospray ionization tandem mass spectrometric method(RP-HPLC/MS2) was developed for the analysis and identification 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-water 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 obtained.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.

【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)
  • 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2007年04期
  • 【分类号】O657.63
  • 【被引频次】15
  • 【下载频次】481
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