文献资料(修改稿).doc

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1、文献资料(修改稿)　　Separationofmicrocystinsandnodularinsbyultraperformanceliquidchromatography超高效液相色谱法分离微囊藻毒素和节球藻毒素LisaSpoof,Milla-RiinaNeffling,JussiMeriluotoAbstractFourultraperformanceliquidchromatography(UPLC)columnswithdifferentreversed-phasecharacteristicsweretestedinthechromatographicsep

2、arationof10microcystinsandthreenodularins,cyanobacterialpeptidetoxins.Thecolumnshadbeendesignedbythemanufacturertowithstandtheultra-highpressuregeneratedbysub-2μmstationaryphaseparticlesandtheWatersACQUITYUPLCsysteminultra-fastseparations.Thegradientmobilephaseconsistedofwaterandacetoni

3、trile,bothacidifiedwithtrifluoroaceticacid,withthreegradientrisetimes:1,1.5and2min.TheUVdetectionofthetoxinswasperformedbyaphotodiodearraydetector.Thechromatographicperformancewasevaluatedbothvisuallyandbycalculatingchromatographicparameterssuchascapacityfactor,resolution,peakwidthathal

4、fheight,selectivityandpeakasymmetry.ThebestchromatographicperformanceasjudgedbyvisualinspectionwasgivenbytheACQUITYBEHShieldRP18andACQUITYBEHPhenylcolumns.TheBEHShieldRP18columnshowedexcellentselectivityandresolutionofchosenpeakpairsconsideredascritical.AfurtheradvantageoftheUPLCsystemw

5、asthehighsamplethroughputwithatotalanalysistimeof3.12min(injection-to-injection)equallingto461separationsper24h.通过对十种微囊藻毒素、三种节球藻毒素和蓝藻毒素肽的色谱分离，我们测试了具有四种不同反相特征的超高效液相色谱（UPLC）柱。　　制造商设计这些柱体能够承受低至2μm的固定相颗粒和沃特世公司ACQUITYUPLC系统快速分离过程中产生的超高压。　　梯度流动相由水和乙腈组成，这两种介质在三种梯度上升时间下——1分钟，1.5分钟和2分钟，都可被三氟乙酸酸化

6、。　　毒素的紫外检测在光电二极管阵列检测器内进行。　　色谱性能通过目视和色谱参数计算评估，色谱参数计算包括容量因子、溶解度、半高峰宽峰、选择性和峰不对称性。　　通过目视的最佳色谱性能是由ACQUITYBEHShieldRP18柱和ACQUITYBEHPhenyl柱得到的。　　ACQUITYBEHShieldRP18柱在被认为是关键的选定峰对的决定上，表现了良好的选择性。　　UPLC系统的另一个更长远的优势在于全程用时达3.12分钟所分析出的高通量（？）样品等同于每24小时分离461个样品。　　1.IntroductionMicrocystinsandnodularin

7、sarecyanobacterialsecondarymetaboliteswhichhavebeencharacterizedasstronghepatotoxinsandtumourpromoters[1].Whenatoxiccyanobacterialmassourrence,bloom,developsinawaterbodythewaterqualityoftendeterioratestoalevelnotaeptableforrecreationalpurposesorfordrinkingwaterabstraction.Micro