简介:摘要:目的:建立一个用液相色谱-质谱联用法测定中药材中黄曲霉毒素含量的方法。方法:色谱柱:thermo Scientific Hypersll GOLDTM(1.9μm,2.1×100mm);流动相: 乙腈-10mmol/L的甲酸铵水溶液,梯度洗脱;流量: 0.3 ml/min;以三重四极杆串联质谱仪检测;柱温:25 ℃。结果:根据药材基质的不同,优化得出相应满足方法要求的前处理方法并进行了验证。结论:该方法可用于中药材中黄曲霉毒素含量的测定。
简介:摘要:目的 采用超高液相色谱配备三重四级杆质谱仪(UPLC-MS/MS)法测定阿那曲唑中痕量杂质偶氮二异丁腈(azodiisobutyronitrile,AIBN)的含量。方法 采用 HICHROM RPB X608色谱柱(3.2mm×100mm,5μm),梯度洗脱,流动相A为甲酸-水(0.2:100,v/v),B为甲酸-甲醇(0.2:100,v/v),(0—0.80min,B 20%—40%;0.80—4.00min,B 40%;4.00—4.10min,B 40%—20%;4.10—5.00min,B 20%),流速1.0 mL·min ,进样量10μL,采用电喷雾离子源(ESI),在正离子模式下选择 m/z 69的分子离子进行检测。结果 AIBN 浓度在6.017~601.6ng·mL 内与峰面积线性关系良好(r=1.000);检测限为1.805ng·mL ,定量限为6.017ng·mL ,样品中杂质 AIBN 测定结果的重复性良好,RSD(n=6)为2.1%;杂质AIBN低、中、高浓度的加样回收率分别为97.3%,96.2%,97.5%,RSD(n=9)为1.71%。经检测,阿那曲唑供试品中AIBN未检出。结论 本方法专属性强,结果准确,灵敏度高,可用于阿那曲唑原料药中AIBN的检测。
简介:摘 要:本文建立了一种通过UPLC-MS/MS测定定西宽粉中米酵菌酸含量的快速检测方法。样品经甲醇-氨水溶液提取后,过0.22µm有机滤膜,上UPLC-MS/MS测定。结果表明,米酵菌酸的质量浓度在1~100ng/mL范围内与色谱峰面积的线性关系良好,R 为0.9996,检出限1.0µg/kg。RSD小于5%(n=6),加标回收率在60%-120%之间。该方法处理样品简单、快捷、检出限低、精密度高,定性、定量准确。
简介:摘要:随着近几年来我国社会各方面的建设发展,科学水平的高速发展正在逐渐开始促进现如今我国社会各行各业的创新进步与发展,并且现代人民群众的生活水平与质量日益提升,对于生活中所面临的诸多方面要求也逐渐开始有所提高,比如人们的衣食住行等问题,在现代经济富足的环境影响下,人们更加重视起食品的安全性来,并且现代食品中经常会发现较多的有害化合物与添加剂,对现代人民群众的健康造成了严重的威胁。基于此,将LC-MS/MS技术应用于食品质量与安全研究中,对现代我国社会食品安全方面的问题做出保障。
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:AbstractBackground:The human brain is the most complex organ in the body, and it is important to have a better understanding of how the protein composition in the brain regions contributes to the pathogenesis of associated neurological disorders.Methods:In this study, a comparative analysis of the frontal and temporal cortex proteomes was conducted by isobaric tags of relative and absolute quantification (iTRAQ) labeling and two-dimensional liquid chromatography-tandem mass spectrometry (2D LC-MS/MS). Brain protein was taken from relatively normal tissue that could not be avoided of damage during emergent surgery of the TBI (traumatic brain injury) patients admitted in Beijing Tiantan Hospital from 2014 to 2017. Eight cases were included. Four frontal lobes and 4 temporal lobes proteome were analyzed and the proteins were quantitated. Gene Ontology (GO), Ingenuity Pathway Analysis (IPA), and Kyoto Encyclopedia of Genes and Genomes (KEGG) pathway analysis were used to analyze the biological function of identified proteins, unchanged proteins, and differentially expressed proteins (DEPs).Results:A total number of 2127 protein groups were identified in the frontal and temporal lobe proteomes. A total of 1709 proteins could be quantitated in both the frontal and temporal cortex. Among 90 DEPs, 14 proteins were screened highly expressed in the temporal cortex, including MAPT, SNCG, ATP5IF1, GAP43, HSPE1, STMN1, NDUFS6, LDHB, SNCB, NDUFA7, MRPS36, EPDR1, CISD1, and RALA. In addition, compared to proteins expressed in the frontal cortex, 14 proteins including EDC4, NIT2, VWF, ASTN1, TGM2, SSB, CLU, HBA1, STOM, CRP, LRG1, SAA2, S100A4, and VTN were a low expression in the temporal cortex. The biological process enrichment showed that unchanged proteins between the frontal and temporal cortex mainly take part in regulated exocytosis, axon guidance, and vesicle-mediated transport. The KEGG pathway analysis showed that unchanged proteins between the frontal and temporal cortex mainly take part in oxidative phosphorylation, carbon metabolism, Huntington's disease, and Parkinson's disease.Conclusions:The majority of proteins are unchanged between the frontal and temporal cortex, and unchanged proteins are closely related to its function. Among DEPs, MATP (tau) is upregulated in the temporal cortex, closely related to Alzheimer's disease (AD), and is one of the targets for the treatment of AD. CLU is downregulated in the temporal cortex which functions as an extracellular chaperone that prevents aggregation of non-native proteins. It was suggested that the temporal lobe may not be the "functional dumb area" of the traditional view, but could be involved in important neural metabolic circuits.
简介:目的:采用HPLC-MS/MS法分析鉴定罗通定在大鼠胆汁中的主要代谢产物。方法:罗通定灌胃给予大鼠(120mg·kg^-1),收集胆汁样品。色谱分离采用ZorbaxSBC18(150mm×0.5mmI.D.,5μm);流动相:甲醇-水-三乙胺(30:70:0.07,V/V/V);质谱分析采用(+)ESI模式。结果:在大鼠胆汁中观察到4个罗通定代谢产物,初步推测其中2个为罗通定去甲基化后再与硫酸结合的产物。结论:去甲基化后形成硫酸结合物为罗通定在大鼠胆汁中一主要排泄形式。
简介:Panaxnotoginsengsaponins(PNS)arethemajorcomponentsofPanaxnotoginseng,withmultiplepharmacologicalactivitiesbutpoororalbioavailability.PNScouldbemetabolizedbygutmicrobiotainvitro,whiletheexactroleofgutmicrobiotaofPNSmetabolisminvivoremainspoorlyunderstood.Inthisstudy,pseudogerm-freeratmodelswereconstructedbyusingbroad-spectrumantibioticstovalidatethegutmicrobiota-mediatedtransformationofPNSinvivo.Moreover,ahighperformanceliquidchromatography-electrosprayionizationtandemmassspectrometry(HPLC-ESI-MS/MS)wasdevelopedforquantitativeanalysisoffourmetabolitesofPNS,includingginsenosideF1(GF1),ginsenosideRh2(GRh2),ginsenosidecompoundK(GCK)andprotopanaxatriol(PPT).Theresultsshowedthatthefourmetabolitescouldbedetectedinthecontrolratplasma,whiletheycouldnotbedeterminedinpseudogerm-freeratplasma.TheresultsimpliedthatPNScouldnotbebiotransformedeffectivelywhengutmicrobiotawasdisrupted.Inconclusion,gutmicrobiotaplaysanimportantroleinbiotransformationofPNSintometabolitesinvivo.
简介:Inthispaper,thebasicconditionsandcharacteristicsoftheDatong-Yanggaoearthquakearedescribedindetail.Thetypeoftheearthquake,theaftershockactivity,theearthquaketrend,thecharacteristicsofdamageareanalyzedanddiscussed.Thisearthquakebelongstoasequenceofearthquakeswarmtypeandisoftheconcentratedlyoccurringcharacteristicsofseveralmainshocksinatimesequence,andtheaftershockactivitywasnormallyattenuated.Becauseoftheunreasonabledesignofbuildingsandrepeatedvibrationbyseveraldestructivemainshockswithinashortperiod,thedamageinthehighintensityregionwasaggravated.Theanalysisandthepredictionprocedureofthe1991Datong-Yanggaoearthquake(Ms=5.8)arealsobrieflygiven.
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。