简介:目的建立超快速液相色谱-质谱/质谱联用(UFLC—MS/MS)法测定酚酞片中酚酞的量。方法样品以乙醇提取、微孔滤膜滤过、离心后,通过电喷雾离子化(ESI),采用多反应检测(MRM)方式进行正离子检测,用于定量分析的检测离子为m/z319.0→225-2。采用Shim-packXR-ODS色谱柱(75mm~3.0mm,2.0μm)分离,以乙腈-水.甲酸(55:45:0.1)为流动相,体积流量为0.40mL/min,在3min内完成酚酞定量分析。结果线性范围为2.5~1000.0ng/mL,最低检测限为2.5ng/mL;日内RSD小于1.85%,日问RSD小于2.56%。结论本方法灵敏度高,分析速度快,操作简单,可作为酚酞片中酚酞质量控制方法。
简介:建立了多反应监测法测定化妆品中α-萘酚和β-萘酚2种禁用着色剂的高效液相色谱-二级质谱联用(HPLC-MS/MS)的分析方法.针对几类美妆用品进行了样品前处理、色谱分离条件和二级质谱条件的研究.色谱条件经优化后确定:以常用的反相键合的十八烷基为固定相,以乙腈和水的二元流动相进行梯度洗脱,以配有电喷雾离子源的二级质谱为检测器等.考察了膏霜类、油状液体类和水类不同基质化妆品中两种萘酚异构体的加标回收率,标准偏差和变异系数.在0.05-10.0mg/L的范围内,2种目标物均有良好的线性关系,检测限(S/N≥10)均为0.2ng/g.6个样品的高、中、低3个标准添加水平下,回收率为81.95%-98.30%,相对标准偏差为0.0015%-0.078%,变异系数为0.83%-8.2%.样品中均未发现禁用着色剂萘酚的2种异构体.该方法可用于化妆品中α-萘酚和β-萘酚的检测.
简介:AIM:ToestablishamethodtosimultaneouslydeterminethemainfivealkaloidsofCatharanthusroseusfortracesamples,ahigh-performanceliquidchromatography–electrosprayionization-tandemmassspectrometry(HPLC-ESI-MS/MS)analysismethodwasdeveloped.METHOD:ThefiveCatharanthusalkaloids,vinblastine,vincristine,vinleurosine,vindoline,andcatharanthinewerechromatographicallyseparatedonaC18HPLCcolumn.Themobilephasewasmethanol-15nmol?L–1ammoniumacetatecontaining0.02%formicacid(65:35,V/V).ThequantificationofthesealkaloidswasbasedontheMultipleReactionMonitoring(MRM)mode.RESULTS:Thismethodwasvalidated,andtheresultsachievedtheaimsofthestudy.Theintra-andinter-dayprecisionandaccuracyofthefivealkaloidswerewithin1.2%-11.5%(RSD%)and-10.9%-10.5%(RE%).Therecoveryratesofthefivealkaloidsofsampleswerefrom79.9%to91.5%.Thefiveanalyteswerestableatroomtemperaturefor2h,at4°Cfor12h,andat-20°Cfortwoweeks.ThedevelopedmethodwasappliedsuccessfullytodeterminethecontentofthefivealkaloidsinthreeplantpartsofthreebatchesofC.roseuswithaminuteamountcollectedfromthreeregionsofChina.CONCLUSION:TheHPLC-ESI-MS/MSmethodcanbeusedforthesimultaneousdeterminationoffiveimportantalkaloidsintraceC.roseussamples.
简介:目的研究甲磺酸桂哌齐特在人尿中的主要代谢产物。方法选择健康受试者12名,连续5d单剂量静脉滴注甲磺酸桂哌齐特250mg,分段收集0~24h尿样,经蛋白沉淀纯化后,直接采用液相色谱-串联质谱法(HPLC-MS/MS)对尿样进行测定。结果在尿样中鉴定出5个主要代谢物,分别为3-O-去甲基-桂哌齐特-葡萄糖醛酸化物(M1)、3-O-去甲基-桂哌齐特-磺酸化物(M2)、桂哌齐特-吡咯烷衍生物(M3)、桂哌齐特-吡咯烷羧基化物(M4)和3-O-去甲基-桂哌齐特(M5)。结论该方法灵敏、选择性高,为深入研究甲磺酸桂哌齐特在人体内的代谢规律提供了可靠的方法。
简介:为建立红枣中氯吡脲(4-CPPU)和赤霉酸(GA3)两种植物生长调节剂残留的高效液相色谱-质谱方法(HPLC-MS),用甲醇超声波提取法提取,经Sep-pakRVac3cc(200mg)C18固相萃取小柱净化,使用AgilentSBC18色谱柱(50mm×2.1mm,1.8μm)分离,在电喷雾离子源(ESI)多反应监测(MRM)离子扫描模式下做HPLCMS检测。试验结果表明:在建立的检测方法条件下,氯吡脲和赤霉酸均在10~100ng/mL检测范围呈线性关系,相关系数均大于0.99;氯吡脲和赤霉酸的检出限均为7ng/mL,定量限分别为22ng/mL和25ng/mL,平均回收率分别为88.5%和93.3%,平均相对标准偏差分别为3.7%和3.8%,达到检测要求。该方法可用于红枣中氯吡脲和赤霉酸的残留测定。
简介:AnM_S7.3earthquakeoccurredonFebruary12,2014inYutianCounty,XinjiangUygurAutonomousRegion,whichwasfollowedbyaseriesofaftershocks.ThispapercalculatesthedepthoftheM_S7.3earthquakesequencebyusingthedeterministicapproachwiththeseismicphasedatafromthecatalogdatabaseoftheChinaEarthquakeNetworksCenter,combinedwithoriginalseismicwaverecordsfromtheDigitalSeismicNetworkCenteroftheEarthquakeAdministrationofXinjiangUygurAutonomousRegion.
简介:ThispapercalculatesthestaticCoulombstresschangesgeneratedbyfourearthquakesintheYutianareaduring2008~2014separately,thendiscussesthetriggeringinfluence,theiraccumulatedCoulombstresschangesandtheirinfluenceonnearbyfaults.TheresultsindicatethattheMS5.5earthquakein2011andtheM_S7.3earthquakein2014arebothintheregionswheretheCoulombstresschangeispositive,thestresschangesare0.004MPaand0.021MPa,respectively,meaningtheyaretriggeredbypriorearthquakes.TheMS6.2earthquakein2012occurredintheplacewhereCoulombstresschangewasnegative,soitispostponedbythepriorearthquakes.TheimageofCoulombstresschangesoftheMS7.3earthquakein2014isinaccordwithaftershocks(ML≥3.0)distribution,butsomeregionsonthefaultwheretheCoulombstresschangeispositivehavefewaftershocks,andstrongaftershocksmayoccuratthesedistrictsinfuture.Inaddition,thispapercalculatestheCoulombstresschangeonnearbyfaults,andfindsthattheCoulombstresschangesofdifferentelementsintheGGCfaultareverydifferent,andmustreceivestrongtriggered-influence,thoughtheresultmaybeinfluencedbytheinputfinitefaultmodel,sothereisstillalargeearthquake-risk.TheGGN,PLC,PLWandLBWfaultswerealsotriggeredbythefourearthquakesoccurringbetween2008~2014.TheirmaximumCoulombstresschangesallexceed0.002MPa,sotheyalsohaveastrongearthquakehazard.
简介:目的:分析安徽亳菊两种栽培类型(大亳菊、小亳菊)挥发油的化学成分,为其质量评价提供科学依据。方法:采用水蒸气蒸馏法提取大亳菊和小亳菊挥发油,用GC毛细管色谱柱进行分析,归一化法测定其相对含量,GC-MS法鉴定化学成分并进行比较。结果:从大亳菊、小亳菊挥发油中分别检出193和237个色谱峰,分别鉴定出51和63个化合物,分别占挥发油总量的75.53%和78.68%。结论:2种亳菊栽培类型挥发油中共有成分为樟脑烯、1-辛烯、6-庚烯-2-醇2,6-二甲基、dl-柠檬烯、沉香醇、filifolone、d-葑醇、(S)-顺式-马鞭草烯醇、菊油环酮、异柠檬醛、马鞭草烯醇、龙脑、α-松油醇、菊烯酯醋酸盐、马鞭草酮、去氢香橙烯、β-紫罗兰酮、α-石竹烯、β-倍半水芹烯和杜松脑。相对含量最高的是马鞭草酮,在大亳菊和小亳菊中的含量分别是14.52%和8.73%;α-石竹烯和β-倍半水芹烯也有一定的含量。亳菊栽培类型不同,挥发油中化学成分在数量上和在种类上都有明显区别,结果为安徽亳菊栽培类型的确立提供了化学方面的佐证,亦为其质量评价提供了物质基础。
简介:摘要目的为鉴定口腔鳞癌的血清标志物和病理分型提供依据。方法采用表面增强激光解吸电离飞行时间质谱(SELDI-TOF-MS)技术及其配套的金芯片(GoldChip)对30份腺癌及健康人30份计60份血清,进行蛋白质谱指纹图分析,筛选口腔鳞癌的差异蛋白。结果在口腔鳞癌患者血清中有3个高表达,m/z(质荷比)分别是9194.06Da,11681.15Da和51370.19Da,应用数据建立分类树模型,获得了一个由7个蛋白9194.06Da,51370.1Da,15879、1Da,6624.57Da,8929.80Da,1l681.1Da,1013.77Da组成的标志蛋白组合模式。在训练组中,该模型的敏感性和特异性分别为92%和96%。结论该模型对诊断口腔鳞癌具有较高的灵敏度和特异度,值得临床应用。
简介:TheYutianearthquakewithM_S7.3happenedonFebruary12,2014.Theprecursormonitoringabilityisweakinthatarea.Wefoundtendencyanomaliesandmiddle-andshort-termanomaliesfrommetalpendulumtiltmeasurementsinHotanseismicstationbeforetheearthquake.AndwealsocomparedtheanomalieswiththatoftheM_S7.3YutianearthquakeonMarch21,2008.Thetendencyanomaliesmeasuredbythemetalpendulumtiltmeterappearedsince2012astiltingeastward.Whilethemiddle-andshort-termanomalieswerecharacterizedbyacceleration,pauseandrapidchangeoftiltrateintwodirections.Thetendencyanomaliesofmetalpendulumtiltrecordsarethesamebeforethetwoearthquakes.Theybothhappenedintheeastdirection.However,therearedifferencesinduration,characteristicandearthquakeintervalsforthemiddle-andshort-termanomalies.
简介:Thedensebroadbandseismicnetworkprovidesmorehigh-qualitywaveformthatishelpfultoimproveconstraintfocaldepthofshallowearthquake.Manyshallowearthquakesoccurringinsedimentwereregardedasinducedevents.InSichuanbasin,gasindustryandsaltminingaredependentonfluidinjectiontechniquethattriggersmicroseismicity.WeadoptedwaveforminversionmethodwithregionalrecordstoobtainfocalmechanismofanMs4.8earthquakeatChangning.TheresultsuggestedthattheChangningearthquakeoccurredataESEthrustfault,anditsfocaldepthwasabout3km.ThedepthphasesincludingteleseismicpPphaseandregionalsPLphaseshowsthatthefocaldepthisabout2km.Thestrong,shortperiodsurfacewavesuggeststhatthiseventisaveryshallowearthquake.TheamplituderatiobetweenRayleighwaveanddirectSwavewasalsousedtoestimatethesourcedepthofthemainshock.Thefocaldepth(2–4km)isfarlessthanthedepthofthesedimentarylayerthickness(6–8km)inepicentralregion.Itisclosetothedepthoffluidinjectionofsaltmining,whichmayimplythatthiseventwastriggeredbytheindustrialactivity.
简介:沙棘籽油样品经微波消解处理,采用电感耦合等离子体质谱法测定所得样品溶液中铁、硒、锌、钾、钠、钙、镁、铜、锰、铅、砷、汞、镉等13种微量元素的含量。使用动态反应池技术消除了多原子离子对部分被测元素的干扰。方法快速准确、灵敏度高,加标回收率在95.5%~102.8%之间,相对标准偏差小于3%。
简介:Thispaperintroducesthegeologicalstructurebackgroundaroundthe2014YutianM_S7.3earthquakearea,investigatesandanalyzestheregimeofsmallearthquakeactivityandthecharacteristicsofregionalseismicitypatterninXinjiangbeforetheearthquake,andcomparesthecharacteristicsoftheregionalseismicactivitywiththe2008YutianM_S7.3earthquake.Theresultsshow:12~3yearsbeforethe2014YutianM_S7.3earthquake,Xinjiangwasinaseismicactivestatewithstrongearthquakeoccurringsuccessively,andbeforethe2008M_S7.3earthquake,Xinjiangwasinthequietstateofmoderate-smallearthquakeswithM3.0~4.0.2BeforethisYutianM_S7.3earthquake,theregionalseismicactivityshowedashort-termanomalyfeature,thatis,seismicityofM≥5.0earthquakessignificantlyincreasedontheAltunseismiczoneandinthesourceareathreeyearsbeforetheM_S7.3earthquake,whileafiveyearlongquiescenceofseismicityofM≥4.0earthquakesappearedontheeastofthesourceareainarangeofabout440km.SixmonthsbeforethisM7.3earthquake,thereexistedseismicgapofM3.0~4.0earthquakesandnear-conjugateseismicbeltmagnitude3.0and4.0inthesourcearea.3ThestateofstrongearthquakeactivityandtheseismicitypatternofsmallearthquakesbeforethisYutianM_S7.3earthquakeweresignificantlydifferenttothatbeforethe2008YutianM_S7.3earthquake,andthismayberelatedtothedifferentseismogenicenvironmentsofthetwoM_S7.3earthquakes.