分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2009年
12期
1815-1819
,共5页
于清峰%肖莹%倪坤仪%Steven Y. Qian
于清峰%肖瑩%倪坤儀%Steven Y. Qian
우청봉%초형%예곤의%Steven Y. Qian
双高-γ-亚麻酸%脂质过氧化%自旋捕集%液相色谱-电子自旋共振波谱联用%液相色谱-质谱联用
雙高-γ-亞痳痠%脂質過氧化%自鏇捕集%液相色譜-電子自鏇共振波譜聯用%液相色譜-質譜聯用
쌍고-γ-아마산%지질과양화%자선포집%액상색보-전자자선공진파보련용%액상색보-질보련용
Dihomo-γ-linolenic acid%lipid peroxidation%spins trapping%liquid chromatography/electron spin resonance%liquid chromatography/mass spectrometry
采用液相色谱-电子自旋共振波谱(LC/ESR)联用技术、液相色谱-质谱(LC/MS)联用技术结合自旋捕集技术,研究了脂氧合酶(LOX)催化双高-γ-亚麻酸(DGLA)脂质过氧化过程中产生的碳自由基.以α-[4-吡啶基-1-氧]-N-叔丁基氮酮(POBN)为自旋捕集剂,在LOX-DGLA反应混合物中与碳自由基形成自旋加合物后,根据各加合物在LC/UV/ESR和LC/MS中对应的保留时间,确定加合物的分子量,进一步根据加合物质谱裂解方式确定其结构.结果表明,在LOX催化DGLA脂质过氧化过程中产生的碳自由基主要包括~·C_7H_(13)O_2,~·C_(10)H_(17)O_2和~·C_5H_(11),分别来自DGLA脂氧自由基(8-,11-,15-LO~·)的β-裂解.此结果有利于进一步研究DGLA在体内的脂质过氧化过程及该过程中产生的碳自由基的生理作用.
採用液相色譜-電子自鏇共振波譜(LC/ESR)聯用技術、液相色譜-質譜(LC/MS)聯用技術結閤自鏇捕集技術,研究瞭脂氧閤酶(LOX)催化雙高-γ-亞痳痠(DGLA)脂質過氧化過程中產生的碳自由基.以α-[4-吡啶基-1-氧]-N-叔丁基氮酮(POBN)為自鏇捕集劑,在LOX-DGLA反應混閤物中與碳自由基形成自鏇加閤物後,根據各加閤物在LC/UV/ESR和LC/MS中對應的保留時間,確定加閤物的分子量,進一步根據加閤物質譜裂解方式確定其結構.結果錶明,在LOX催化DGLA脂質過氧化過程中產生的碳自由基主要包括~·C_7H_(13)O_2,~·C_(10)H_(17)O_2和~·C_5H_(11),分彆來自DGLA脂氧自由基(8-,11-,15-LO~·)的β-裂解.此結果有利于進一步研究DGLA在體內的脂質過氧化過程及該過程中產生的碳自由基的生理作用.
채용액상색보-전자자선공진파보(LC/ESR)련용기술、액상색보-질보(LC/MS)련용기술결합자선포집기술,연구료지양합매(LOX)최화쌍고-γ-아마산(DGLA)지질과양화과정중산생적탄자유기.이α-[4-필정기-1-양]-N-숙정기담동(POBN)위자선포집제,재LOX-DGLA반응혼합물중여탄자유기형성자선가합물후,근거각가합물재LC/UV/ESR화LC/MS중대응적보류시간,학정가합물적분자량,진일보근거가합물질보렬해방식학정기결구.결과표명,재LOX최화DGLA지질과양화과정중산생적탄자유기주요포괄~·C_7H_(13)O_2,~·C_(10)H_(17)O_2화~·C_5H_(11),분별래자DGLA지양자유기(8-,11-,15-LO~·)적β-렬해.차결과유리우진일보연구DGLA재체내적지질과양화과정급해과정중산생적탄자유기적생리작용.
A combination technique of LC/ESR, LC/MS and spin trapping was used to identify and characterize the carbon-centered free radicals formed from lipoxygenase-catalyzed peroxidation of dihomo-γ-linolenic acid(DGLA). The spin trap, α-[4-pyridyl-1-oxide]-N-tert-butyl nitrone(POBN), could react with short-lived carbon-centered radicals to form relatively stable adducts. Based on the same retention time of POBN radical adduct in LC/UV/ESR and LC/MS, molecular weight of adduct could be confirmed and the structure of adduct could be confirmed by their LC/MS2 fragment pattern. The results showed that free radicals formed in lipoxygenase-catalyzed peroxidation of DGLA, including ~·C_7H_(13)O_2, ~·C_(10)H_(17)O_2 and ~·C_5H_(11), all stemmed from β-scission of DGLA alkoxyl radicals(8-, 11-, 15-LO~·). The results were helpful for further study of biological activities of these radicals in vivo.