简介:目的运用高效液相色谱-高分辨飞行时间质谱联用(HPLC-TOF-MS)技术和高效液相色谱串联三重四级杆质谱(HPLC-MS/MS)法,对产复康颗粒化学成分进行快速鉴定及定量分析,并进行初步药动学研究。方法HPLC-TOF-MS法采用ZORBAXEclipsePlusC18(100mm×3.0mm,1.8μm)色谱柱;流动相为乙腈(A)-0.1%甲酸水(B),梯度洗脱,体积流量0.2mL/min;质谱采用正、负离子扫描,扫描范围m/z100~2000。HPLC-MS/MS法采用WatersXBridge?BEHC18(150mm×4.6mm,2.5μm)色谱柱;流动相为乙腈(A)-0.1%甲酸水(B),梯度洗脱,体积流量0.4mL/min;ScheduledMRM正负离子切换监测模式定量分析。ig给予SD大鼠产复康颗粒(0.5、5g/kg),给药后于不同时间点颈静脉取血0.2mL,分离血浆,HPLC-MS/MS法检测产复康颗粒入血成分及含量。结果HPLC-TOF-MS法鉴定产复康颗粒中24种成分;建立的HPLC-MS/MS方法分离度良好,各方法学验证均符合要求,对13种主要成分进行定量分析,水苏碱、黄芪甲苷和益母草碱的含量较高,可能是其主要活性成分;药动学结果显示,仅在给药剂量5g/kg时,血浆中可检测到水苏碱和益母草碱,水苏碱的消除较慢,益母草碱快速消除。结论该方法简便、准确,重复性好,可用于产复康颗粒中多种成分的鉴定和含量的测定,为药材的质量控制、药动学研究提供了参考。
简介:摘要 : 目的:以 MALDI- TOF MS 为代表的蛋白质谱技术在微生物检验和科研中的应用 分析 。方法:文献检索及实际应用分析。结果:基质辅助激光解吸电离飞行时间质谱 (MALDI- TOF MS) 是一种软电离质谱,适用于分析蛋白质等生物大分子物质,可用来绘制微生物的蛋白质图谱,最终可达到鉴定目的。基于 MALDI-TOF MS 的蛋白质谱技术具有快速、准确、敏感性高、高通量等特点,目前已应用于细菌和真菌的鉴定,结论: MALDI-TOF MS 在微生物分型、耐药性分析等领域的应用初有成效,具有很大的应用发展空间。
简介:AristolochiaeFructus,aChineseherbalmedicinederivedfromthefruitofAristolochiacontortaBge.,containsnephrotoxicaristolochicacidanalogues(AAAs).Accordingtoancientmedicaltexts,variousmedicinalpartsofthefruitofA.contortawereeverused.Inordertorevealwhichpartcouldbesafelyandeffectivelyused,itisnecessarytoanalyzethechemicalprofilesofdifferentmedicinalparts.HereinwecomparedthechemicalcompositionsanddeterminedaristolochicacidI(AA-I)andaristolochicacidII(AA-II)inthefourpartsviz.outerpericarp,innerpericarp,septum,andseed.Ultra-highperformanceliquidchromatographyequippedwithquadrupoletime-of-flightmassspectrometry(UHPLC-QTOF-MS)wasappliedforchemicalprofiling.Ultra-highperformanceliquidcoupledwithtriplequadrupolemassspectrometry(UHPLC-QqQ-MS)wasemployedtoquantifyAA-IandAA-IIindifferentparts.Itwasfoundthatthechemicalcompositionsofthefourpartsvariedbothqualitativelyandquantitatively.Atotalof10AAAs,including5aristolochicacidsand5aristolactams,togetherwith3alkaloids,wereunambiguouslyortentativelyidentifiedbyUHPLC-QTOF-MS.ThequantitativelyanalyticalresultsobtainedbyUHPLC-QqQ-MSshowedthatAA-IandAA-IIexclusivelyaccumulateintheseedsofA.contorta.Thesefindingsprovidesupportingdatafortherationalselectionofmedicinalparts.
简介:目的:采用UPLC/Q-TOF-MS技术对玫瑰花渣中的黄酮类成分进行定性分析。方法:采用WatersBEHC18色谱柱(100mm×2.1mm,1.7μm),柱温:40℃,洗脱系统为乙腈-0.1%甲酸水梯度洗脱;采用ESI离子源并在负离子模式下进行采集数据。结果:通过UPLC的快速分离,根据质谱数据并结合文献分析推测,鉴定了11种黄酮类化合物。结论:采用UPLC/Q-TOF-MS技术,可有效地分析玫瑰花渣中黄酮类成分,为玫瑰花渣的回收利用提供了数据支持。
简介:建立灵敏、高效、可重复的HPLC-MS/MS法测定人血浆中己烯雌酚的浓度。血浆经乙酸乙酯蛋白沉淀,黄豆苷元为内标,使用AgilentC18色谱柱(4.6mm×150mm,5μm),以乙腈–2.5mM醋酸铵水溶液(60:40,v/v)为流动相,通过电喷雾离子化四极杆串联质谱,负离子多反应检测模式(MRM),用于定量的离子反应分别为m/z267.2→237.3(己烯雌酚)、m/z253.2→132.3(黄豆苷元)。己烯雌酚浓度为0.1–20ng/mL时线性关系良好(r~2=0.9984),该方法的重复性实验RSD为4.7%,准确度为90%–105%,最低检测限为0.1ng/mL。该方法重现性好,定量限低,适用于检测药物己烯雌酚的血药浓度并进行药代动力学研究。
简介:Theearthquakestress-dropvaluesoftwosequenceswereaccuratelycalculatedaftertakingawaytheeffectsduetoregionalearthquakeanelasticattenuationandstationsiteresponse,usingwaveformdataandseismicphasedataofsequencesoftheJingguM_S6.6,andLudianM_S6.5earthquakesinYunnan.Theseresultsshowthatthestressdropwithmagnitudeincreaseswithinthescopeofthisstudyofmagnitude.Aftereliminatingtheinfluenceofthemagnitude,theaveragevalueofstress-dropintheJinggusequenceishigherthanthatoftheLudiansequenceatthesamemagnituderange.Thismayberelatedtothestressstateindifferentregions.Intermsofthechangesoftimeandspaceofstress-drop,beforeM_S5.8strongaftershock,thestress-dropis'slowingdown-turningup-keepingahighvalue'afterthemainshock,meanwhile,almostalloftheabnormallyhighstressdropvalueisdistributedaroundtheM_S5.8strongaftershock,showingthatthestressenvironmentintheregionwasincreasingafterthemainshock.AndaftertheM_S5.9strongaftershock,stress-droprapidlydeclinestoarelativelystablestate,meanwhile,thehighvalueofstress-dropisdistributedaroundthestrongaftershock,showingthattheregionaltectonicstressgetsmorefullyrelease,itsstressenvironmentbeginstorapidlydecrease.FortheLudiansequencewithoutastrongaftershockoccurring,theaveragevalueofstressdropislowerthanthatoftheJingguearthquakesequenceatthesamemagnituderange,whileatthesametime,thestress-dropoftheaftershocksequencealmosthasn'tchangedmuch.Inthetimeafterthemainshock,combinedwiththereleasecharacteristicsofthemainenergy,thestressintheregionisexcessivelyreleased,thesubsequentstressintheregiongraduallyreturnstonormal.ThismaybethereasonwhytheactivityofLudianaftershockssignificantlywasweakerandsubsequentlytherewerenostrongaftershocksoccurred.
简介:目的:建立超高效液相色谱三重四极杆串联质谱法(UPLC-MS/MS)同时测定不同产地吊石苣苔中4个苯乙醇苷类成分的方法,分析比较不同产地吊石苣苔中苯乙醇苷含量差异。方法:采用ACQUITYUPLCBEHC18色谱柱(100mm×2.1mm,1.8μm);以0.1%甲酸-水(A)-0.1%甲酸乙腈(B)溶液为流动相,梯度洗脱,体积流量为0.5mL·min^-1;柱温为40℃,采用电喷雾离子源,负离子检测方式,得到相应的提取离子流图。结果:不同产地吊石苣苔中4个苯乙醇苷含量有明显差异,结论:该方法操作简便、准确、重复性好,对寻找高含量苯乙醇苷的资源植物及产地具有重要的理论指导意义。
简介:摘要水质安全检测在环境安全监测中占有重要的一环,然而,电感耦合等离子体质谱(ICP-MS)技术由于其低检出限、多元素同时分析等优点被广泛应用于水质检测中。据此,ICP-MS法在水中总汞测定的探究显得非常重要。本文对ICP-MS在测定水中汞中的应用进行了简要分析。
简介:本研究以贵州省黔东南自治州黎平县野生亮叶含笑为研究对象。采用水蒸气蒸馏法对亮叶含笑的8种不同器官(即一年生叶,一年生茎,两年生茎,花瓣,雄蕊,雌蕊,苞片,假种皮)进行精油提取,并使用GC-MS与峰面积归一化法分离、分析其化学成分与相对含量。结果表明:亮叶含笑8种器官的精油中共检测出52种化合物,大多属于倍半萜类,有部分单萜类和萜类含氧的衍生物,属于酸酯类的化合物。亮叶含笑叶一年生中含有14种化合物;一年生茎含有16种化合物;两年生茎含有14种化合物;假种皮含有19种化合物;花含有24种化合物;苞片含有16种化合物。不同的器官的精油化合物的种类存在一定差异。
简介:通过对单糖甲基化产物裂解原理的分析,将气相色谱-质谱法(GC/MS)裂解产生的片段分为母片段、二级片段、高级片段及特征片段四类;分析了四类片段在定性分析中不同的作用及应采用的比对方式.归纳总结了先比对特征片段,再比对母片段离子和次级片段离子的比对定性方法,为提高单糖甲基化GC/MS片段定性准确性提供了依据.
简介:目的建立UPLC-MS/MS法检测中成药及保健品中非法添加的10种抗风湿类化学成分的含量。方法以ACQUITYUPLCBEHC18(50mm×2.1mm,1.7μm)为色谱柱,以含0.1%乙酸0.02mol/L醋酸铵溶液-乙腈为流动相梯度洗脱,体积流量为0.3mL/min;质谱采用电喷雾离子源(ESI),多反应监测(MRM)模式进行定性定量分析。结果10种化学物质的质谱检测线性范围宽,线性关系良好,r≥0.9961,平均方法回收率为92.5%~101.8%,RSD为0.9%~3.1%,检出限为0.0015~0.018μg,定量限为0.0045~0.55μg,27批样品中有10批样品检出了非法添加的化学物质。结论本方法操作简单,灵敏度高,结果准确,可作为抗风湿类中成药及保健品中非法添加化学物质的测定方法。
简介:TheJuly3,2015PishanM_S6.5earthquakeoccurredintheintersectionareaoftheTarimblockandWestKunlunblockwherethemoderate-strongearthquakeshavebecomeactiveinrecentyears.Thispaperhasstudiedtheseismicityparametersoftheearthquakesequencessuchastheb-valueinthePishanregionanditsvicinity.Inaddition,wealsorelocatedtheaftershocksofthePishanM_S6.5earthquakeusingtheseismicphasereportbythedouble-differencemethod.ThetemporalandspatialvariationcharacteristicsofthePishanearthquakesequenceintherupturezoneareanalyzed.Thestudyisofgreatsignificanceintheseismichazardassessmentinthisregion.
简介:Inthispaper,statisticsaretakenontheco-seismicresponseofundergroundfluidinYunnantotheNepalM_S8.1earthquake,andtheco-seismicresponsecharacteristicsofthewaterlevelandwatertemperatureareanalyzedandsummarizedwiththedigitaldata.TheresultsshowthattheNepalM_S8.1earthquakehadgreaterimpactontheYunnanregion,andthemacroandmicrodynamicsoffluidsshowedsignificantco-seismicresponse.Theearthquakerecordingcapacityofwaterlevelandtemperaturemeasurementissignificantlyhigherthanthatofwaterradonandwaterqualitytothislargeearthquake;themaximumamplitudeanddurationofco-seismicresponseofwaterlevelandwatertemperaturevarygreatlyindifferentwells.Thechangingformsaredominatedbyfluctuationandstepriseinwaterlevel,andarisingorfallingrestorationinwatertemperature.Fromtherecordsofthemainshockandthemaximumstrongaftershock,wecanseethatthegreatermagnitudeofearthquake,thehigherratiooftheoccurrenceofco-seismicresponse,andinthesamewell,thelargertheresponseamplitude,aswellasthelongertheduration.Theamplitudeanddurationofco-seismicresponserecordedbydifferentinstrumentsinasamewellaredifferent.Watertemperatureco-seismicresponsealmostoccurredinwellswithwaterlevelresponse,indicatingthatthewellwaterlevelandwatertemperaturearecloselyrelatedinco-seismicresponse,andthewellwatertemperatureseismicresponsewascausedmainlybywellwaterlevelseismicresponse.
简介:为避免精油因加热时间过长造成热解使某些芳香成分破坏,本文采用恒压漏斗代替传统的水蒸气蒸馏装置提取薰衣草精油,在单因素实验基础上通过正交试验探讨薰衣草精油的最佳提取工艺条件,研究结果表明:料液比为1∶6,提取时间1.5h,浸泡时间1h时,薰衣草精油出油率最高,可达1.15%;对提取出的薰衣草精油进行GC/MS测定,共检测出33个组分,其中有7种组分含量较高,依次是芳樟醇,含量为54.57%,乙酸芳樟醇,为14.38%,4-萜烯醇,为8.96%,乙酸薰衣草酯,为8.94%,异龙脑,为6.19%,α-松油醇,为4.31%,薰衣草醇,为2.65%。该实验装置简单,操作简便,绿色环保,并且提取效果理想,结果可靠,可为其他精油的提取提供参考。
简介:采用微波消解法对花草茶样品进行前处理,利用电感耦合等电子体质谱仪(ICP-MS)同时测定了样品中As、Cd、Cr、Pb、Sr、Mn、Cu、Zn等8种金属元素的含量。结果表明,采用微波消解-ICP-MS法的测得加标回收率为92.6~101.3%,实验结果满足检验要求,适用于花草茶中多种元素的同时快速确证检测。且该前处理方法相比干化法,检测时间更短,结果更准确。
简介:ThefruitsofPaulowniacatalpifoliaGongTongareusedasaChinesefolkherbalmedicineforthetreatmentofenteritis,tonsillitis,bronchitis,anddysentery,etc.OurpreviousstudyhasidentifiednewC-geranylatedflavanoneswithobviousanti-proliferativeeffectsinlungcancerA549cells.Inthepresentstudy,anewC-geranylatedflavone,paucatalinoneC(1)andfiveknownC-geranylatedflavanones(2-6)wereisolated.Inaddition,atotalof34C-geranylatedflavonoidsweredetectedbyHPLC-DAD-ESI-MS/MScouplingtechniquesfromtheCH_2Cl_2extractofP.catalpifolia.Futhermore,anti-agingeffectsofisolatedcompoundswereevaluatedinvitrowithprematuresenescent2BScellsinducedbyH_2O_2.PhytochemicalresultsindicatedthatP.catalpifoliawasanaturalresourceofabundantC-geranylatedflavonoids.Diplacone(3)andpaucatalinoneA(5)werethepotentanti-agingagentsintheprematuresenescent2BScellsinducedbyH_2O_2andtheC-geranylsubstituentmaybeanimportantfactorbecauseofitslipophiliccharacter.