《农业相关翻译》由会员分享，可在线阅读，更多相关《农业相关翻译（2页珍藏版）》请在金锄头文库上搜索。
1、Qualitativeanalysis定性分析Determinationoftheretentiontimesforeachintactglucosinolatestandard每个完整的硫代葡萄糖苷的标准保留时间的测定IntheHPLCanalysis,thetwelveintactglucosinolatestandardswerebaselineseparatedasshowninFigure4.Themostpolarglucosinolatestandard,glucoiberinwasfirstelutedout.WhenthecompositionofmobilephaseBwa
2、sincreasedbythegradientprogram,therelativelynon-polarglucosinolateswereelutedoutinanorderofdescendingtheolaritiesoftheglucosinolatestandards.Themostnon-polarglucosinolatestandard,luconasturtiinwasthelastonetobeelutedout在高效液相色谱分析，12个完整的硫代葡萄糖苷的标准，如在图4所示的基线分离。大多数极性苷的标准，glucoiberin首先被洗脱出来。当流动相B组成的梯度程序增加
3、，相对非极性的硫代葡萄糖苷洗脱为了降的硫代葡萄糖苷的标准的olarities。最非极性苷标准，luconasturtiin是最后一个被洗脱出来。UnderthechromatographicconditionsdescribedinChapter2.7,theaverageandrelativeretentiontimesforeachglucosinolatestandardweredeterminedandshowninTable6:在第2.7章所述的色谱条件下，平均每个苷标准和相对保留时间进行了测定，并在表6所示：Identificationoftheglucosinolatesinve
4、getableandTraditionalChineseMedicine(TCM)samplesbyusingreversed-phaseHPLCanalysis采用反相高效液相色谱法分析蔬菜和中医(TCM)样品中的硫代葡萄糖苷的鉴定TheglucosinolatesinthreevegetableandtenTCMsampleswereanalyzed.Bycomparingtheretentiontimesofthesampleextractswiththoseoftheglucosinolatestandards,thepresenceoftheglucosinolatesinthesa
5、mpleextractscouldbeidentified.However,theretentiontimesoftheglucosinolatesinthesampleextractsvariedalittlebitduetothecomplicatedmarticesinthesampleextracts.Therefore,asmallvolumeof1,000ppmglucosinolatemixturestandardsolutionwasspikedintothesampleextractsfortheidentificationoftheglucosinolatesinthesa
6、mpleextracts.Bycomparingthepeakareasofthecorrespondingretentiontimesinthechromatogramoforiginalsampleextractwiththespikedone,thepeakareasofthespikedonewereincreased.Itidentifiedthatthesampleextractcontainedtheglucosinolatesbeingspiked.Byrepeatingthespikedstandardmethoddescribedabove,itidentifiedthat
7、RootofIsatisindigoticaFort.北板藍根containedglucoiberin,glucocheirolin,progoitrin,sinigrin,epiprogoitrin,glucoraphenin,sinalbin,gluconapin,glucotropaeolin,glucoerucinandgluconasturtiin.ThechromatogramsofRootofIsatisindigoticaFort.北板藍根extractandRootofIsatisindigoticaFort.北板藍根extractwithstandardsspikedwer
8、eshowninFigures5aand5brespectively.三种蔬菜和10个中药样品中的硫代葡萄糖苷进行了分析。苷标准的样品提取物的保留时间比较，可确定样本中提取的硫代葡萄糖苷的存在。然而，提取不同样品中的硫代葡萄糖苷的保留时间由于样本中提取的复杂martices的一点点。因此，1000ppm的硫代葡萄糖苷的混合标准溶液的体积小，被添加到的样本中提取的硫代葡萄糖苷的鉴定的样品提取。在与飙升的原始样本中提取相应的保留时间的色谱峰面积比较，加标峰面积均增加。它确定了样品提取中正在飙升的硫代葡萄糖苷。重复上面介绍的方法加标标准，确定了板蓝根的根。北板藍根所载glucoiberin，gluc
9、ocheirolin，progoitrin，sinigrin，epiprogoitrin，glucoraphenin，sinalbin，gluconapin，glucotropaeolin，glucoerucin和gluconasturtiin。菘蓝根的色谱。北板藍根板蓝根提取物和根。北板藍根标准飙升提取物分别在图5a和5b所示。IdentificationoftheglucosinolatesinvegetableandTraditionalChineseMedicine(TCM)samplesbyusingESI-QTOF-MSandMS/MSanalysis蔬菜和中医(TCM)样品中的硫
10、代葡萄糖苷使用ESI-QTOF-MS和MS/MS分析鉴定ByusingthespikedstandardmethoddescribedinChapter3.1.2,theglucosinolatesinthesampleextractscanbedetected.However,theretentiontimesofthespikedglucosinolatestandardsmightbesameasthoseoftheinterferencesinthesampleextracts.Topinpointtheco-elutionproblemmentionedabove,theelectr
11、osprayionzation-quadrupoletime-of-flightmassspectrometryinnegativemodewasusedforfurtherconfirmationoftheHPLCfractionsoftheglucosinolatesdetectedinthesampleextracts.Theidentificationwasbasedonthemolecularionmassandthepatternoftheircorrespondingfragmentions.Itwasamorepowerfulmethodthanthespikedstandar
12、dmethodandcapableofprovidingtheinformationontheelementalcompositionsandthestructuresofthemolecules.HPLCfractionsoftheglucosinolatesdetectedinvegetableandTCMsampleextractwerecollected.Thecollectedfractionsweredilutedwithmethanol,followedbynegativeESI-QTOF-MSanalysis.Thedeprotonedmolecularion,M-H-ofth
13、eHPLCfractioninESI-QTOF-MSspectrumwascomparedwiththatofthecorrespondingglucosinolatestandard.Forexample,thedeprotonatedmolecularion,M-H-ofgluconapinstandardwasfoundtobem/z372.0536inESI-QTOF-MSspectrum.Bycomparingthemassofthedeprotonatedmolecularion,M-H-ofthegluconapinstandardwiththatoftheRootofIsati
14、sindigoticaFort.北板藍根extractat11.883min,m/z372.0233wasfound.ItshowedapositiveresultforthefurtherconfirmationofthegluconapinintheHPLCfractioncollectedfromtheRootofIsatisindigoticaFort.北板藍根extractat11.883min.TheESI-QTOF-MSspectrumsofgluconapinstandardandRootofIsatisindigoticaFort.北板藍根extractat11.883min
15、wereshowninFigure6aand6brespectively.通过加标章3.1.2中所述的标准方法，可检测样品中提取的硫代葡萄糖苷。然而，飙升苷标准的保留时间，可能是样本中提取的干扰一样。为了查明的合作洗脱上述问题，在负离子模式电ionzation四极杆飞行时间质谱用于检测样本中提取物的硫代葡萄糖苷的HPLC组分的进一步确认。识别是基于分子离子的质量和其相应的碎片离子的格局。这是一个更有效的方法比飙升的标准方法，并能够提供的元素组成和分子结构的信息。蔬菜和中药样本提取物中检测到的硫代葡萄糖苷的高效液相色谱馏分收集。收集馏分，用甲醇稀释，负ESI-QTOF-MS分析。deprotoned分子离子MH-HPLCESI-QTOF-MS谱分数与相应的硫代葡萄糖苷的标准相比,，例如，去质子化分子离子MH-gluconapin标准被发现的m/z372.0536ESI-QTOF-MS谱。通过比较去质子化的分子离子的质量，Hgluconapin标准与板蓝根的根。北板藍根11.883min提取物，M/Z372.0233被发现。它显示为阳性结果进一步证实板蓝根的根从收集到的高效液相色谱分数gluconapin。北板藍根提取11.883min。gluconapin标准ESI-QTOF-MS谱和板蓝根根。北板藍根在11.883min提取物，分别在图6a和6b所示。
