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1、2007年7月色谱Vo.l25No.4July2007ChineseJournalofChromatography524~527L-羟脯氨酸寡肽混合物的高效液相色谱分离与质谱分析11122,3孙艳亭,卢奎,马丽,曹书霞,赵玉芬(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;3.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
2、物的色谱分离条件。实验以YWGC8柱(10m,250mm10mm)为分离柱,以乙腈-006%三氟乙酸水溶液(体积比为298)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。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中图分类号:O658文献标识码:A文章编号:1000-8713(2007)04-0524-04栏目类别:研究论文IsolationandIdentificationoftheMixtu
3、reofL-HydroxyprolineOligo-PeptidesbyReversed-PhaseHighPerformanceLiquidChromatographyandElectrosprayIonizationTandemMassSpectrometry11122,3SUNYanting,LUKui,MALi,CAOShuxia,ZHAOYufen(1.SchoolofChemistryandChemicalEngineering,HenanUniversityofTechnology,Zhengzhou450052,China;2.K
4、eyLaboratoryforChemicalBiology,DepartmentofChemistry,ZhengzhouUniversity,Zhengzhou450052,China;3.DepartmentofChemistry,XiamenUniversity,Xiamen361005,China)Abstract:Areversed-phasehighperformanceliquidchromatographic-electrosprayionization2tandemmassspectrometricmethod(RP-HPLC
5、/MS)wasdevelopedfortheanalysisandident-ificationofareactionmixtureofL-hydroxyprolineoligo-peptides.ThemixturewasseparatedonaYWGC8column(10m,250mm10mm)usingacetonitrile-watercontaining0.06%triflu-oroaceticacid(298,v/v)asthemobilephase.Theseparationconditionswereoptimized.Th
6、emixturewasanalysedwithelectrosprayionizationmassspectrometry(ESI-MS)andESI-2MS/MSinpositivemode.MSandMSspectraofindividualchromatographicpeakwereob-tained.Itindicatedthattherewerehydroxyprolinedipeptide,hydroxyprolinetripeptideandhydroxyprolinecyclo-dipeptideinthemixtures,be
7、sideshydroxyproline.Thedescribedmethodcanbeeffectivelyappliedtoperformidentificationofhydroxyprolineoligo-peptidemixtures.Keywords:reversed-phasehighperformanceliquidchromatography(RP-HPLC);electrosprayionizationtandemmassspectrometry(ESI-MS/MS);L-hydroxyprolineoligo-pep-tide
8、mixture寡肽类化合物一般具有较强的生物活性,多数对其进行分离纯化,以最终获得高纯度的产品。随[1]可作为药物或药物前体,因此如