简介:摘要:目的 建立UPLC-MS/MS法同时测定大败毒胶囊中的芍药苷、绿原酸、橙皮苷3个成分的含有量。方法 Agilent poroshell 120 EC-C18(2.1mm×50mm,1.9μm)色谱柱,流动相A为乙腈,流动相B为0.02%甲酸水溶液,梯度洗脱,柱温为35℃,流速为0.2ml/min,进样量为5μl;电喷雾(ESI)离子源。结果 各组分在线性范围内线性关系良好,平均加样回收率98.1%-102.1%,RSD1.83%-4.42%。结论 该方法结果准确可靠,效率高,可为大败毒胶囊的质量控制研究提供科学依据。
简介:摘要目的评价血清分离胶促凝管法和HB&L微生物培养体系两种MALDI-TOF-MS预处理方法的鉴定率,为临床快速准确鉴定血流感染病原菌提供新思路。方法收集2020年1—12月北京解放军总医院第六医学中心实验室常规方法鉴定的149份血培养报警后单一细菌感染的阳性样本,分别采用分离胶促凝管法和HB&L微生物培养体系预处理后,并且以传统方法结果为标准,直接MALDI-TOF MS细菌鉴定,比较两种方法的鉴定率。结果在149份血培养阳性样本中,革兰阴性(G-)菌占47.0%(70/149)、革兰阳性(G+)菌占53.0%(79/149)。对G-菌种水平鉴定率,血清分离胶促凝管法为78.6%(55/70),HB&L微生物培养体系为91.4%(64/70),差异有统计学意义(P=0.033);对G+菌种水平鉴定率,二者分别为73.4%(58/79)和87.3%(69/79),差异有统计学意义(P=0.028)。在3.000~2.300分值段,G-菌鉴定率血清分离胶促凝管法和HB&L微生物培养体系分别为22.9%(16/70)和38.6%(27/70),差异有统计学意义(P=0.044);G+菌鉴定率两种方法分别为19.0%(15/79)和34.2%(27/79),差异有统计学意义(P=0.031)。结论HB&L微生物培养体系种水平鉴定率要高于血清分离胶促凝管法,经过预处理直接MALDI-TOF MS鉴定血培养阳性样本病原菌有一定临床应用价值。
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:摘要: 目的 采用UHPLC-MS/MS法测定中成药中西地那非、伐地那非、他达那非。方法 采用Agilent C18 (1.8μm,2.1×50mm) 色谱柱;流速:0.2mL/min ;流动相: A为含0.1%乙酸的0.02mol/L乙酸铵溶液,B相为甲醇,梯度洗脱;柱温35℃。结果 三种物质在所建立的色谱条件下均能较好分离, 在 20ng/mL~200ng/mL浓度范围内线性关系良好,相关系数均大于0.995,平均回收率97.3%~102.0%。结论 该方法前处理简单、选择性强,灵敏度高,可用于测定中成药中3种非法添加的壮阳类化学药物。
简介:摘要:建立了一种全新的以QuEChERS法为样品前处理技术结合UPLC-TQS法快速测定动物源性食品多种兽药残留的方法。样品经甲醇-乙腈混合溶液提取并通过DISQUETM净化管净化,上清液经正己烷除去脂肪、样品浓缩后用色谱柱进行分离,以甲醇5mmol/L醋酸铵含0.1%甲酸水溶液为流动相进行梯度洗脱,多反应监测(MRM)模式检测,外标法定量。结果表明:目标物在1~50μg/kg的空白添加浓度范围内均有良好线性关系,相关系数r≥0.99;样品中多种药物的检出限(LOD)均为0.5μg/kg,定量限(LQD)均为1.0μg/kg;在5~20μg/kg的添加水平范围内平均回收率为75.8%~93.2%,(RSD)为3.1%~13.2%。该方法具备快速、简便、准确性高、用性强等特点,适合动物源性食品中多类药物残留的定性定量检测。
简介:摘要:本文建立了一种利用液相色谱-串联质谱法LC-Ms/Ms测定蜂产品中氯霉素残留量的方法。样本提取、净化后,经乙腈-水流动相体系洗脱,C18色谱柱分析后,利用三重四级杆液相色谱质谱联用仪灵敏度高、专属性强、定量准确来检测氯霉素,可以用来快速筛查蜂蜜和蜂王浆中的氯霉素残留。
简介:摘要目的探讨零回波时间磁共振血管成像(zero echo time MR angiography,ZTE-MRA)及时间飞跃法磁共振血管成像(time of fight MR angiography,TOF-MRA)的图像质量以及对脑动脉狭窄诊断的价值。材料与方法纳入19例拟诊断为脑动脉狭窄的患者,同时进行ZTE-MRA及TOF-MRA检查,以数字减影血管造影(digital subtraction angiography,DSA)作为金标准,评估两种MRA成像技术诊断脑动脉狭窄的准确度、敏感度、特异度。结果ZTE-MRA和TOF-MRA的优良图像占比和信噪比(signal-to-noise ratio,SNR)平均值分别为84%、74%和14.2、19.4,差异均无统计学意义(P=0.583、0.175);诊断脑动脉狭窄ZTE-MRA的敏感度和特异度为100%和98%,TOF-MRA相应为85%和96%,ZTE-MRA的Kappa值为0.898优于TOF-MRA;ZTE-MRA诊断1~2级动脉狭窄和3~4级动脉狭窄准确度分别为57%和81%。TOF-MRA相应为46%和31%。诊断1~2级动脉狭窄差异无统计学意义(P=0.427),3~4级狭窄差异具有统计学意义(P=0.017)。结论ZTE-MRA和TOF-MRA的图像质量无明显差异,两者对于1~2级脑动脉狭窄诊断价值无差别,对于3~4级脑动脉狭窄ZTE-MRA较TOF-MRA更为准确。
简介:【摘要】目的:探讨多层螺旋CT血管造影(MSCTA)、3D-TOF磁共振血管成像(MRA)在颈动脉狭窄诊断中的价值。方法:回顾性分析2018月10月至2020年10月60例颈部血管狭窄并行DSA检查的神经内科住院患者的临床资料,分别行CTA和MRA检查,以DSA检查结果为金标准,评价CTA和MRA对颈动脉狭窄的诊断价值。结果:64 MS-CTA检出142处狭窄,其中54处轻度,72处中度,13处重度,3处闭塞。3D TOF-MRA 150处狭窄,其中59处轻度,73处中度,14处重度,4处闭塞;3D TOF-MRA提示147支病变血管,与DSA诊断符合率达93.9%,64 MS-CTA提示142支病变血管,与DSA诊断符合率达97.2%;结论:MSCTA、3D-TOF MRA均能较准确诊断颈动脉狭窄,但各有优缺点,二者结合可以从多方面来诊断颈部血管狭窄性病变,可以成为脑血管疾病筛查方法。
简介:摘要:本论文旨在建立运用电感耦合等离子体质谱技术同时检测水中25种元素含量的方法。除铍、硼两个待测元素运用No gas调谐模式,其余23种待测元素均运用He模式消除测定中的质谱干扰,同时应用在线添加内标液的形式校正非质谱干扰,提高测定方法的灵敏度和准确度。本实验所测25种待测元素质量浓度线性关系较好,标准曲线相关系数R在0.9994~1.0000。本方法建立的水中25种待测元素的检出限为0.00127~7.58μg/L,相对标准偏差RSD%在0.2%~4.6%,三个不同加标浓度水平下测试的水样平均加标回收率为87.5%~129%。本实验所建方法具有线性范围宽,较高的灵敏度、精密度和准确度,满足水中25种元素痕量检测和定量分析的要求。
简介:摘要 目的:对延边州地区10批朝鲜当归中重金属元素铅(Pb)、镉(Cd)、砷(As)、汞(Hg)、铜(Cu)进行测定。方法:样品制备采用微波消解法,测定采用电感耦合等离子体质谱(ICP-MS)法。结果:铅、砷在0~20ng/ml,镉在0~10ng/ml,铜0~500ng/ml,汞0~5ng/ml范围内与各自CPS比值呈良好的线性关系,铅、砷、镉、铜、汞的回归方程分别为y=0.0093X-0.0012,y=0.0051X+0.003895,y=0.0061X+0.006473,y=0.1276X-0.00363,y=0.0024X+0.0045733,r均为0.9999,精密度、稳定性、重复性试验结果的RSD均<5%,平均回收率分别为
简介:摘要:多环芳烃 Polycyclic Aromatic Hydrocarbons;PAHs