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Massspectrometry
AnAgilentXCTPlusiontrapmassspectrometer
(ITMS)(AgilentTechnology,US)wasusedtoanalyze
thefractions,Fr.1–10,obtainedfromethylacetate
extracts.Atmosphericpressurechemicalionization
(APCI)MSwasperformedinthepositivemode.The
drygasandvaporisertemperatureswere350and
4008C,respectively.
FortheanalysisofCP1,Electrospray-Ionization
MassSpectrometry(ESI-MS)wasperformedusinga
WatersMicromassQ-Tofmicromassspectrometer
(Waters,USA).Samplewasdirectlyinfusedataspeed
of10ml/minforacquiringmassspectra.Thecapillary
andsampleconevoltagesweremaintainedat3.0kV
and50V,respectively.Thesourceanddesolvation
temperatureswere80and2508C,respectively.The
massspectrawereacquiredfromm/z100to5000in
thepositiveionmode.
Nuclearmagneticresonancespectrometry(NMR)
TheNMRspectraofcompound1,CP1andCP2
wererecordedonaBrukerAdvanceAMX500NMR
spectrometer(Rheinstetten,Germany)at500.13MHz
113
(H)and125.75MHz(C),respectively.Tetramethyl-
silane(TMS)wasusedasaninternalstandard.
Compound1wasdissolvedinmethanol-d4;CP1and
CP2weredissolvedinD2O.
Statisticalanalysis
Themeanvalueswerecalculatedfromdatataken
fromatleastthreeseparateexperiments.Where
significancetestingwasperformed,aStudent’st-test
wasused;P-valuesof,0.05wereconsideredtobe
statisticallysignificant.
Results
NosignificantdifferencesinTEACvalueorHPLC
profileweredetectedbetweendifferentbottlesofthe
samecommercialbatch.Theantioxidantcomponents
inDSSwerefoundtobestableduring1–2months
storage,basedontheTEACvalueandtheirHPLC
profile.
Separationandcharacterizationoflowmolecularmass
components
DSSwasextractedwithmethanol,andthemethanol
ext
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