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Super Antibiotics, Part II. Hyperforin, Mass Spectroscopy (MS) and Gas Chromatography-Mass Spectrometry (GC-MS), Evidence of Permeability of the Blood-Testis Barrier (BTB) and the Blood-Brain Barrier (BBB) to Hyperforin 被引量:2
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作者 Ilia Brondz 《International Journal of Analytical Mass Spectrometry and Chromatography》 2016年第4期66-73,共8页
In the first article of this series, we presented some evidence of hyperforin as an antibiotic, antiprotozoal, antiviral, anticancer, and immunomodulatory substance. In the present article, evidence of the permeabilit... In the first article of this series, we presented some evidence of hyperforin as an antibiotic, antiprotozoal, antiviral, anticancer, and immunomodulatory substance. In the present article, evidence of the permeability of the blood-testis barrier (BTB) and blood-brain barrier (BBB) to hyperforin and its distribution in other organs of the domestic pig (Sus scrofa domesticus) are revealed. Seven-month-old male boars with a body mass of 100 kg were fed a diet containing hyperforin. Organs were surgically removed under anesthesia. Organs were suitable prepared and extracted, and then analyzed using gas chromatography-mass spectrometry with supersonic molecular beams (GC-MS with SMB). The presence of hyperforin was recorded in all organs and body fluids. Special attention was paid to the evaluation of the presence of hyperforin in the brain and testes of experimental animals. The presence of hyperforin in the brain and testes of experimental animals was established by GC-MS with SMB. The results are of interest because penicillin and numerous other antibiotics cannot pass through the BTB or BBB if healthy or non-inflamed, which limits their use in patients with meningitis and gonorrhea. The findings are also of interest in cases of penicillin- and multi-antibiotic-resistant bacterial infections. 展开更多
关键词 ANTIBIOTICS HYPERFORIN Super antibiotic Mass Spectroscopy Gas Chromatography-Mass spectrometry blood-Testis Barrier blood-Brain Barrier Methicillin-Resistant Staphylococcus aureus (MRSA)
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碰撞/反应池电感耦合等离子体质谱(ICP-MS)法测定血液中16种元素
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作者 于宏洋 王萌 +3 位作者 汪冰 王娟 李孟楠 胡克 《中国无机分析化学》 CAS 北大核心 2024年第1期131-138,共8页
采用直接稀释法,使用电感耦合等离子体质谱仪测定血液中元素的过程中,由于血液样本成分复杂,容易产生较大的基体效应,同时一系列多原子离子(例如,^(40)Ar^(16)O^(+)、^(40)Ar^(40)Ar^(+)等)会影响与其有相同质荷比核素的检测,进而影响... 采用直接稀释法,使用电感耦合等离子体质谱仪测定血液中元素的过程中,由于血液样本成分复杂,容易产生较大的基体效应,同时一系列多原子离子(例如,^(40)Ar^(16)O^(+)、^(40)Ar^(40)Ar^(+)等)会影响与其有相同质荷比核素的检测,进而影响测定结果。通过使电感耦合等离子体质谱仪(ICP-MS)分别工作在标准模式、氦气模式和氢气模式下,对比仪器的氧化物离子产率(CeO/Ce)、双电荷离子产率(Ba^(++)/Ba)、灵敏度与检出限情况,同时对氢气模式时仪器上述指标优于其他两种模式的潜在机理进行分析;随后再使用氢气作为碰撞/反应池气体,使用直接稀释法分析全血标准品以及小鼠血液样本中16种元素的含量情况。结果表明,使用氢气作为碰撞/反应池气体时,氧化物离子产率(CeO/Ce)、双电荷离子产率(Ba^(++)/Ba)、灵敏度与检出限情况优于标准模式和氦气模式,且16种元素在0.5~100.0μg/L线性关系良好(R2≥0.99991),对全血标准品中分析准确度为86.0%~114%,分析小鼠血液样本时的加标回收率为81.2%~115%,仪器精密度为2.3%~4.8%,使用氢气作为电感耦合等离子体质谱仪技术的碰撞/反应池气体,为分析血液样品中16种元素(V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ge、As、Se、Cd、Hg、Tl、Pb、Bi)开发一种新的分析方法,也为血液金属组学分析提供了新方法。 展开更多
关键词 电感耦合等离子体质谱仪 碰撞反应池 血液金属组学
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发育性颈椎管狭窄人群血清差异蛋白质组学分析
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作者 卜献忠 钟远鸣 +5 位作者 卜保献 李记天 汪利合 李慧英 杨汉立 许伟 《中国组织工程研究》 CAS 北大核心 2024年第34期5432-5439,共8页
背景:正常健康人与发育性颈椎管狭窄(气虚血瘀证)人群之间的血清特异性生物学标志物尚未完全明确。目的:寻找并鉴定气虚血瘀证发育性颈椎管狭窄的潜在生物学标志物。方法:分别采集发育性颈椎管狭窄(气虚血瘀证)人群血清9例、健康正常人... 背景:正常健康人与发育性颈椎管狭窄(气虚血瘀证)人群之间的血清特异性生物学标志物尚未完全明确。目的:寻找并鉴定气虚血瘀证发育性颈椎管狭窄的潜在生物学标志物。方法:分别采集发育性颈椎管狭窄(气虚血瘀证)人群血清9例、健康正常人群血清8例,采用同位素相对标记与绝对定量技术串联质谱标签联合液相色谱-串联质谱筛选2组人群血清的差异蛋白及鉴定,使用Western Blot法对肌球蛋白轻链3(MYL3)差异蛋白进行验证。结果与结论:(1)串联质谱标签技术:共鉴定出61个差异蛋白(P <0.05),其中与健康正常人群组比,补体成分C1q受体、载脂蛋白A4、C-C基序趋化因子配体18等14种差异蛋白明显上调,而肌球蛋白轻链3、线粒体翻译延伸因子、核仁磷酸蛋白1等47种差异蛋白明显下调;(2)基因富集分析:这些差异蛋白可能参与染色体组织、线粒体膜组织、肌肉系统过程的调节等分子功能;(3)蛋白相互作用网络分析:健康正常人群与发育性颈椎管狭窄(气虚血瘀证)人群之间的共同差异蛋白中补体C1q受体、载脂蛋白A4、C-C基序趋化因子配体18、肌球蛋白轻链3、线粒体翻译延伸因子、核仁磷酸蛋白1等38种位于功能网络节点,且与颈椎骨能量代谢、骨细胞产生、破骨细胞的形成等系统关系密切;(4)运用Western Blot法对主要差异蛋白肌球蛋白轻链3进行验证:其验证结果与蛋白组学结果相一致;(5)结论:通过绝对定量技术联合液相色谱-串联质谱技术发现健康正常人群与发育性颈椎管狭窄(气虚血瘀证)人群之间的血清差异表达蛋白,并初步推测肌球蛋白轻链3可能是发育性颈椎管狭窄(气虚血瘀证)人群的特异性血清标志物。 展开更多
关键词 发育性颈椎管狭窄 气虚血瘀证 串联质谱标签 血清蛋白标志物 蛋白组学
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超高效液相色谱-串联质谱法同时测定人血中12种抗抑郁药
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作者 徐峰 宣宇 +5 位作者 卓晓聪 富利祥 陈峰 王斌杰 郭狄飞 余鹏飞 《中国司法鉴定》 2024年第1期53-60,共8页
目的 建立超高效液相色谱-串联质谱法同时测定人血中吗氯贝胺、安非他酮等12种抗抑郁药的分析方法。方法 血液样品经乙腈(含内标普罗地芬)沉淀蛋白后进样测定。采用ACQUITY UPLC HSS T3色谱性(2.1 mm×100 mm,1.8μm)进行分离,以2 m... 目的 建立超高效液相色谱-串联质谱法同时测定人血中吗氯贝胺、安非他酮等12种抗抑郁药的分析方法。方法 血液样品经乙腈(含内标普罗地芬)沉淀蛋白后进样测定。采用ACQUITY UPLC HSS T3色谱性(2.1 mm×100 mm,1.8μm)进行分离,以2 mmol/mL甲酸铵和0.1%甲酸的水溶液-2 mmol/mL甲酸铵和0.1%甲酸的乙腈溶液体系进行梯度洗脱,流速0.35 mL/min。以电喷雾离子源正离子和多反应监测模式进行检测,内标法定量。结果 在相应质量浓度范围内,12种抗抑郁药的相关系数均大于0.999,检出限为0.05~0.2 ng/mL,定量限为0.5~1 ng/mL;在低、中、高不同添加浓度条件下,准确度为-7.1%~11.7%,日内精密度为0.1%~11.5%,日间精密度为1.9%~9.4%,提取回收率为85.7%~113.5%,基质效应为-18.2%~10.2%;各成分在不同添加水平和不同环境下的稳定性为-9.30%~11.30%。综上均符合生物样品分析及法医毒物分析要求。结论 该方法选择性强、重现性好、精密度高,可同时检测人血中12种抗抑郁药,可适用于法医毒物检验鉴定,对非正常死亡案(事)件中死者死因分析具有重要意义。 展开更多
关键词 法医毒物学 超高效液相色谱-串联质谱法 抗抑郁药 人血
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适用于法庭科学毒物分析的干血斑检验体系的建立——以5种常见药(毒)物为例
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作者 苏东斌 董林沛 +2 位作者 张云峰 赵鹏 李开开 《色谱》 CAS CSCD 北大核心 2024年第3期245-255,共11页
干血斑技术能够方便地对血液样品中的违禁药物进行快速分析,在酒后驾驶检查、滥用药物检测、兴奋剂检测等毒物分析场景具有显著优势。然而在我国法庭科学毒物分析领域,因缺少标准化检验体系,其稳定性和可靠性未得到深入研究论证,限制了... 干血斑技术能够方便地对血液样品中的违禁药物进行快速分析,在酒后驾驶检查、滥用药物检测、兴奋剂检测等毒物分析场景具有显著优势。然而在我国法庭科学毒物分析领域,因缺少标准化检验体系,其稳定性和可靠性未得到深入研究论证,限制了其在司法实践中的运用。本研究以甲基苯丙胺、利多卡因、氯胺酮、芬太尼和地西泮为典型药(毒)物,使用整个干血斑进行分析,建立了适用于法庭科学领域毒物分析的超高效液相色谱-串联质谱分析方法,形成了以干血斑样品制作、前处理、分析、储存和效用性评价为主要内容的检验体系,并为干血斑中其他药(毒)物的分析方法开发提供参考。结果表明,干血斑中利多卡因和芬太尼在0.5~100 ng/mL内线性关系良好,甲基苯丙胺、氯胺酮、地西泮在2~100 ng/mL内线性关系良好,方法检出限为0.2~0.5 ng/mL。干血斑中5种目标物可以在60天内保持稳定,目标物测定含量与理论值的偏差在15%以内。干血斑中5种目标物的测量结果与全血一致,没有显著的系统误差和比例误差,芬太尼、地西泮、氯胺酮、利多卡因和甲基苯丙胺的测量浓度的相对偏差分别为4.44%、3.50%、7.66%、5.10%和5.25%。干血斑样品前处理方法简单,样品用量小,能够实现血液样品保存的轻量化和规范化且与全血样品具有高度定量一致性,可为公安实践工作中分析、保存血液检材提供新方案。 展开更多
关键词 超高效液相色谱-串联质谱 毒物分析 干血斑 储存条件 稳定性
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QuEChERS-高效液相色谱-四极杆-飞行时间质谱法正负离子切换同时检测血液中的6种除草剂
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作者 史洪飞 徐伯芃 徐成鑫 《分析科学学报》 CAS CSCD 北大核心 2024年第2期219-224,共6页
建立了基于QuEChERS-高效液相色谱-四极杆-飞行时间质谱法检测血液中草除灵乙酯、二氯吡啶酸、三氯吡氧乙酸、三氟啶磺隆、丙炔氟草胺、硝黄草酮等6种除草剂的分析方法。样品用乙腈涡旋振荡提取,提取液经优化的QuEChERS方法净化,0.22μ... 建立了基于QuEChERS-高效液相色谱-四极杆-飞行时间质谱法检测血液中草除灵乙酯、二氯吡啶酸、三氯吡氧乙酸、三氟啶磺隆、丙炔氟草胺、硝黄草酮等6种除草剂的分析方法。样品用乙腈涡旋振荡提取,提取液经优化的QuEChERS方法净化,0.22μm滤膜过滤。采用ZORBAXEclipse PlusC18色谱柱(100mm×3.0mm,1.8μm),以0.1%甲酸水溶液和乙腈为流动相梯度洗脱实现色谱分离,四极杆-飞行时间质谱正负离子切换检测。结果显示,6种除草剂的线性相关系数均大于0.9981,检出限为0.02~1.95μg/L,定量限为0.07~6.49μg/L;在100μg/kg和500μg/kg两种加标水平下的样品回收率为88.19%~105.19%;仪器精密度为0.39%~1.65%,日内方法精密度为0.81%~2.93%,日间方法精密度为0.08%~2.85%。所建立方法灵敏度高、稳定性强、分析速度快,能够满足血液中除草剂成分的定性、定量分析需要,可为除草剂中毒案件中生物检材的检验提供参考。 展开更多
关键词 高效液相色谱 四极杆-飞行时间质谱法 正负离子切换模式 血液 除草剂
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颈部超声与CT血管造影对颈动脉狭窄病变的诊断价值
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作者 马金龙 刘强 《中国卫生标准管理》 2024年第8期141-145,共5页
目的探讨颈部彩色多普勒超声(color doppler ultrasound,CDUS)与CT血管造影(CT angiography,CTA)对颈动脉狭窄病变的诊断价值。方法回顾性选取2021年1月—2023年6月于松原吉林油田医院就诊的70例缺血性脑血管患者,整理并分析其临床资料... 目的探讨颈部彩色多普勒超声(color doppler ultrasound,CDUS)与CT血管造影(CT angiography,CTA)对颈动脉狭窄病变的诊断价值。方法回顾性选取2021年1月—2023年6月于松原吉林油田医院就诊的70例缺血性脑血管患者,整理并分析其临床资料。所有患者均接受数字减影造影(digital subtraction angiography,DSA)、CDUS、CTA检查。比较CDUS、CTA检出结果、诊断效能、阴性组与阳性组的血流动力学参数、2种检查方式对颈动脉斑块的检出结果,并对其中的典型病例进行分析。结果70例缺血性脑血管患者经DSA检查后,确诊为阳性者21例,阴性49例。经CDUS检查阳性30例,阴性40例,其中仅有17例确诊为颈动脉狭窄病变;经CTA检查,阳性27例,阴性43例,其中仅有20例确诊为颈动脉狭窄病变。CTA检查的准确度更高于CDUS;经比较发现,CTA的颈动脉斑块检出率高于CDUS;差异有统计学意义(P<0.05);2种诊断方式的敏感度与特异度比较,差异无统计学意义(P>0.05);根据DSA检查结果将患者分为阴性组与阳性组,分别49例、21例,阳性组颈内动脉收缩期峰值流速(peak systolic flow velocity of internal carotid artery,PSV)、舒张期末流速(end diastolic flow velocity,EDV)均高于阴性组,大脑中动脉搏动指数(arterial pulsation index,PI)、平均血流速度(average blood flow velocity,Vm)均低于阴性组,差异有统计学意义(P<0.05)。结论相较于CDUS,CTA检测准确性较高,具备一定应用优势,但需注射对比剂,应用范围受到一定局限。CDUS准确性相对较低,但同时具备重复性良好、无创等优势,还可对患者脑部血流状态学进行检测。CTA的颈动脉斑块检出率更高,但斑块分型准确性不高。2种检查方式均具备独特优势,临床应用时可从实际需求出发选择合适的检查方式。 展开更多
关键词 颈动脉狭窄病变 颈部彩色多普勒超声 CT血管造影 数字减影造影 脑部血流状态学 诊断价值
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MALDI-TOF MS与VITEK2在血流感染致病菌快速鉴定及药敏试验中的应用
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作者 邓文 余静贵 +3 位作者 李洁群 赵娜 王玮 胡凯 《赣南医学院学报》 2024年第4期383-391,共9页
目的:探究基质辅助激光解吸/电离飞行时间质谱(Matrix-assisted laser desorption/ionizationtime-of-flight mass spectrometry,MALDI-TOF MS)与VITEK2在血流感染致病菌药敏试验中的联合应用效果。方法:选取景德镇市第二人民医院检验科... 目的:探究基质辅助激光解吸/电离飞行时间质谱(Matrix-assisted laser desorption/ionizationtime-of-flight mass spectrometry,MALDI-TOF MS)与VITEK2在血流感染致病菌药敏试验中的联合应用效果。方法:选取景德镇市第二人民医院检验科2022年1月1日至2022年12月31日血流感染阳性样本126份,分别行常规鉴定及MALDI-TOF MS鉴定,完成菌株鉴定后通过VITEK2系统行抗菌药物敏感性试验(Antimicrobial susceptibility testing,AST),比较2种鉴定方法的细菌菌株鉴定结果及细菌耐药情况。结果:常规鉴定方法对革兰氏阴性、革兰氏阳性菌在属、种水平鉴定符合率达到100%;MALDI-TOF MS鉴定革兰氏阴性菌在属水平的符合率达97.7%(85/87),在种水平的符合率达95.4%(83/87),2例无结果(1例阴沟肠杆菌阴沟亚种,1例少动鞘氨醇单胞菌);MALDI-TOF MS鉴定革兰氏阳性菌在属、种水平的符合率均达97.4%(38/39),1例无结果(科氏葡萄球菌解脲亚种)。常规鉴定+VITEK2对革兰氏阴性菌AST分析的分类一致(Categorical agreement,CA)、基本一致(Essential agreement,EA)分别达到98.6%(1086/1101)、99.5%(1096/1101),对革兰氏阳性菌AST分析的CA、EA分别达到98.6%(550/558)、99.6%(556/558);MALDI-TOF MS+VITEK2(VITEK MS)对革兰氏阴性菌AST分析的CA、EA分别达到98.3%(1082/1101)、99.5%(1095/1101),对革兰氏阳性菌AST分析的CA、EA分别达到97.8%(546/558)、99.5%(555/558)。进一步参考肉汤稀释法药敏结果行一致性分析。结果发现,常规鉴定+VITEK2在革兰氏阴性菌的药敏试验中,10份AST鉴定结果出现小误差(Minus errors,MIE),5份AST鉴定结果出现重大误差(Major errors,ME);在革兰氏阳性菌的药敏试验中,8份AST鉴定结果出现MIE,2份AST鉴定结果出现ME。VITEK MS在革兰氏阳性菌的药敏试验中,13份AST鉴定结果出现MIE,6份AST鉴定结果出现ME;在革兰氏阳性菌的药敏试验中,9份AST鉴定结果出现MIE,3份AST鉴定结果出现ME。结论:MALDI-TOF MS联合VITEK2在临床血流感染致病菌鉴定及药敏试验中可快速、精确实现诊断并提供AST报告。 展开更多
关键词 基质辅助激光解吸/电离飞行时间质谱 血流感染 抗菌药物敏感性试验
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调Q-Nd:YAG激光联合桂枝茯苓汤加减治疗痰瘀互结型玫瑰痤疮疗效分析
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作者 鹿晓兰 李敬果 +6 位作者 唐志铭 单霄 陈桂升 张晓宇 李洁 管志强 丁继存 《内蒙古中医药》 2024年第1期108-111,共4页
目的:评价调Q-Nd:YAG激光联合桂枝茯苓汤加减治疗痰瘀互结型玫瑰痤疮疗效的影响。方法:将纳入研究的129例痰瘀互结型玫瑰痤疮病患者按照随机数表法分为治疗组和对照1.2组。对照1组予以调Q-Nd:YAG激光治疗,对照2组予以桂枝茯苓汤加减治... 目的:评价调Q-Nd:YAG激光联合桂枝茯苓汤加减治疗痰瘀互结型玫瑰痤疮疗效的影响。方法:将纳入研究的129例痰瘀互结型玫瑰痤疮病患者按照随机数表法分为治疗组和对照1.2组。对照1组予以调Q-Nd:YAG激光治疗,对照2组予以桂枝茯苓汤加减治疗。治疗组采用联合治疗方案。统计三组治疗前后各项临床症状[毛细血管扩张面积占比和丘疹(脓疱)以及瘙痒红斑]评分及临床疗效、皮肤病生活质量指数(DLQI)量表评分,并比较三组临床疗效及不良反应情况和复发情况。结果:三组治疗前基本情况差异无统计学意义(P>0.05);治疗组皮损改善明显,有效率达86.0%(37/43),对照组有效率为65.1%(28/43)/60.4%(26/43),与对照1.2组比较差异有统计学意义(P<0.01);治疗组在生活质量改善方面与对照1.2组比较差异有统计学意义(P<0.01)。不良反应方面三组无明显差异(P>0.05)。复发率方面,对照1.2组明显高于治疗组,差异有统计学意义(P<0.01)。结论:调Q-Nd:YAG激光联合桂枝茯苓汤加减治疗痰瘀互结型玫瑰痤疮临床疗效显著,不良反应少且复发率低,值得临床应用。 展开更多
关键词 调Q-Nd:YAG激光 桂枝茯苓汤加减 痰瘀互结型玫瑰痤疮 生活质量指数 丘疹脓疱型
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Use of blood-based biomarkers for early diagnosis and surveillance of colorectal cancer 被引量:11
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作者 Ganepola AP Ganepola Joel Nizin +1 位作者 John R Rutledge David H Chang 《World Journal of Gastrointestinal Oncology》 SCIE CAS 2014年第4期83-97,共15页
Early screening for colorectal cancer(CRC) holds the key to combat and control the increasing global burden of CRC morbidity and mortality. However, the current available screening modalities are severely inadequate b... Early screening for colorectal cancer(CRC) holds the key to combat and control the increasing global burden of CRC morbidity and mortality. However, the current available screening modalities are severely inadequate because of their high cost and cumbersome preparatory procedures that ultimately lead to a low participation rate. People simply do not like to have colonoscopies. It would be ideal, therefore, to develop an alternative modality based on blood biomarkers as the first line screening test. This will allow for the differentiation of the general population from high risk individuals. Colonoscopy would then become the secondary test, to further screen the high risk segment of the population. This will encourage participation and therefore help to reach the goal of early detection and thereby reduce the anticipated increasing global CRC incidence rate. A blood-based screening test is anappealing alternative as it is non-invasive and poses minimal risk to patients. It is easy to perform, can be repeated at shorter intervals, and therefore would likely lead to a much higher participation rate. This review surveys various blood-based test strategies currently under investigation, discusses the potency of what is available, and assesses how new technology may contribute to future test design. 展开更多
关键词 Colorectal neoplasms Early detection of cancer Colonoscopy Biological markers blood Messenger RNA MicroRNA Long NON-CODING RNA DNA methylation MICROSATELLITE instability Loss of HETEROZYGOSITY High-throughput nucleotide sequencing Mass spectrometry Real-time polymerase chain reaction Microarray analysis
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Identification of potential oxidative stress biomarkers for spinal cord injury in erythrocytes using mass spectrometry 被引量:1
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作者 Li-Jian Zhang Yao Chen +2 位作者 Lu-Xuan Wang Xiao-Qing Zhuang He-Chun Xia 《Neural Regeneration Research》 SCIE CAS CSCD 2021年第7期1294-1301,共8页
Oxidative stress is a hallmark of secondary injury associated with spinal cord injury.Identifying stable and specific oxidative biomarkers is of important significance for studying spinal cord injury-associated second... Oxidative stress is a hallmark of secondary injury associated with spinal cord injury.Identifying stable and specific oxidative biomarkers is of important significance for studying spinal cord injury-associated secondary injury.Mature erythrocytes do not contain nuclei and mitochondria and cannot be transcribed and translated.Therefore, mature erythrocytes are highly sensitive to oxidative stress and may become a valuable biomarker.In the present study, we revealed the proteome dynamics of protein expression in erythrocytes of beagle dogs in the acute and subacute phases of spinal cord injury using mass spectrometry-based approaches.We found 26 proteins that were differentially expressed in the acute(0–3 days) and subacute(7–21 days) phases of spinal cord injury.Bioinformatics analysis revealed that these differentially expressed proteins were involved in glutathione metabolism, lipid metabolism, and pentose phosphate and other oxidative stress pathways.Western blot assays validated the differential expression of glutathione synthetase, transaldolase, and myeloperoxidase.This result was consistent with mass spectrometry results, suggesting that erythrocytes can be used as a novel sample source of biological markers of oxidative stress in spinal cord injury.Glutathione synthetase, transaldolase, and myeloperoxidase sourced from erythrocytes are potential biomarkers of oxidative stress after spinal cord injury.This study was approved by the Experimental Animal Centre of Ningxia Medical University, China(approval No.2017-073) on February 13, 2017. 展开更多
关键词 acute phase bioinformatic analysis biomarkers central nervous system DOG erythrocytes mass spectrometry oxidative stress peripheral blood spinal cord injury subacute phase
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Simultaneous Screening for 45 Poisonous Alkaloids in Blood by LC-MS/MS 被引量:1
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作者 ZHAI Jin-xiao SHEN Min LIU Wei 《法医学杂志》 CAS CSCD 2015年第1期28-33,共6页
Objective To develop a liquid chromatography-tandem mass spectrometry(LC-MS/MS) screening method for 45 poisonous alkaloids in blood. Methods Identification was based on the compound's retention time and two precu... Objective To develop a liquid chromatography-tandem mass spectrometry(LC-MS/MS) screening method for 45 poisonous alkaloids in blood. Methods Identification was based on the compound's retention time and two precursor-to-production transitions. The method involved a liquid-liquid extraction(LLE) followed by LC-MS/MS with multiple-reaction monitoring(MRM). When 1 m L of blood was extracted with diethyl ether at p H=9.2 with SKF525 Aas the internal standard, the target compounds were analyzed with LC-MS/MS in the positive ionization mode. Results The target alkaloids had good linearity(r>0.995 1), both the intra-day precision and inter-day precision being less than 14.77%. The limits of detection ranged from 0.05 to 25 ng/m L in blood. Conclusion The method is selective and sensitive in detecting poisonous alkaloids with a total running time of 12 minutes; therefore it was successfully applied to some actual cases of suspected alkaloids poisoning. 展开更多
关键词 法医遗传学 手套 DNA 检验
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HPLC-MS/MS Determination of Oleandrin and Adynerin in Blood with Solid Phase Supported Liquid-Liquid Extraction
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作者 Jianbo YING Fanglin WANG +1 位作者 Yujing LUAN Weixuan YAO 《Medicinal Plant》 CAS 2018年第3期5-8,共4页
[Objectives]To optimize the determination method of oleandrin and adynerin in blood. [Methods]High performance liquid chromatography-mass spectrometry( HPLC-MS/MS) was applied to determine oleandrin and adynerin in bl... [Objectives]To optimize the determination method of oleandrin and adynerin in blood. [Methods]High performance liquid chromatography-mass spectrometry( HPLC-MS/MS) was applied to determine oleandrin and adynerin in blood. The blood sample was dispersed and fixed on a solid phase supported liquid-liquid extraction column and eluted with ethyl acetate. The resulting eluent was used for chromatographic separation with Kinetex C_(18) column as the separation column and gradient elution was performed using 10 mmol/L ammonium formate solution containing 0. 1%( volume fraction) formic acid and acetonitrile as the mobile phase. In the tandem mass spectrometry analysis,the detection was carried out using the electrospray positive ion source multiple reaction monitoring mode. [Results] The mass concentration of oleandrin and adynerin showed linear relationship in the range of 2-100 μg/L. The limit of detection( 3 S/N) of the method was 0. 5 μg/L.A blank sample was used as the substrate for the spike recovery test. The recovery rate was in the range of 90. 0%-98. 0%,and the relative standard deviation( RSD) of the measured values( n = 6) was in the range of 2. 1%-7. 3%. [Conclusions]The method established in this experiment has the benefits of simple pretreatment,good recovery,high sensitivity and strong specificity,and is expected to provide an ideal method for the determination of such drugs in blood. 展开更多
关键词 High performance liquid chromatography-mass spectrometry(HPLC-MS/MS) blood Oleandrin Adynerin
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Determination of Exposure to Medical and Industrial Toxic Chemicals from Beijing by Human Hair, Nail and Blood Analysis
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作者 G. Yang D. Kechkeche +1 位作者 H. Belhadj-Tahar N. Sadeg 《Forensic Medicine and Anatomy Research》 2015年第1期27-31,共5页
The aim of the present work was to investigate the exposure to the medical and industrial toxic chemicals. The research was carried out on hair, nail and blood samples in a panel of 40 healthy volunteers aged 7 to 77 ... The aim of the present work was to investigate the exposure to the medical and industrial toxic chemicals. The research was carried out on hair, nail and blood samples in a panel of 40 healthy volunteers aged 7 to 77 with an average of 45 ± 19 years (18 women (45%) and 22 men (55%)). All of these individuals had not received medication for at least 1 year, including antibiotics and psychotropic. This study was realized from July 2013 to March 2014 in Beijing, China. The method for an accurate and reliable screening of medical and an industrial toxic chemical was based on detection and assay by ultra-high performance liquid chromatography with UV detection type of diode arrays. Also more than 10,000 toxic molecules commonly found in western industrial countries were screened by coupling gas chromatography and mass spectrometry. The main results indicate that the molecules analyzed are mainly antibiotic (Gentamycine and Tobramycine), antidepressant (Amitriptylin and its metabolites), narcotic (MDMA and Clonitazene), ingredient in cosmetics (Benzenediol and Benzoic acid), insecticide (Carbamate derivative), ketamine, chlorhexidine and phthalate derivatives. There are no detailed documented baseline data of the analysis of medical and Industrial toxic pollutants in hair, nail and blood samples in Beijing;however, this study should be completed on samples from other provinces of China. This study is the first of its kind. Therefore, further studies should be conducted in other cities and provinces of China to be compared with each other. 展开更多
关键词 POLLUTANTS HAIR NAIL blood Toxicological SCREENING Separative Method Mass spectrometry
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Chlorpyrifos Determined in Human Blood by UPLC-MS/MS and Its Application in Poisoning Cases 被引量:1
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作者 QIAO Zheng YAN Hui +1 位作者 ZHUO Xian-yi SHEN Bao-hua 《法医学杂志》 CAS CSCD 2015年第2期112-116,共5页
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Method Development and Validation for Determining 1,3-Bu- tadiene in Human Blood by Gas Chromatography-Mass Spec- trometry and Head-Space Gas Chromatography
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作者 ZHANG Su-jing SHEN Bao-hua ZHUO Xian-yi 《法医学杂志》 CAS CSCD 2013年第2期110-115,共6页
To develop a simple,validated method for identifying and quantifying 1,3-butadiene(BD) in human blood by gas chromatography-mass spectrometry(GC-MS) and head-space gas chromatography(HS-GC).BD was identified by GC-MS ... To develop a simple,validated method for identifying and quantifying 1,3-butadiene(BD) in human blood by gas chromatography-mass spectrometry(GC-MS) and head-space gas chromatography(HS-GC).BD was identified by GC-MS and HS-GC,and quantified by HS-GC.The method showed that BD had a good linearity from 50 to 500μg/mL(r>0.99).The limits of detection and quantification were 10 μg/mL and 50 μg/mL,respectively.Both the intra-day precision and inter-day precision were <6.08%,and the accuracy was 96.98%-103.81%.The method was applied to an actual case,and the concentration of BD in the case was 242 μg/mL in human blood.This simple method is found to be useful for the routine forensic analysis of acute exposure to BD. 展开更多
关键词 摘要 编辑部 编辑工作 读者
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超高效液相色谱-四极杆飞行时间质谱法快速定性、定量分析人全血中米酵菌酸
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作者 周丽屏 郭嘉明 +2 位作者 郭尧平 陈纠 王致 《理化检验(化学分册)》 CAS CSCD 北大核心 2023年第2期142-147,共6页
采集疑似米酵菌酸中毒患者全血样品200μL,加入已于-20℃冷冻的甲醇800μL,振荡5 min,离心5 min,上清液按照优化的仪器工作条件分析。在Infinity Lab Poroshell 120 EC-C_(18)色谱柱(150 mm×3.0 mm, 2.7μm)上以不同体积比的含10 m... 采集疑似米酵菌酸中毒患者全血样品200μL,加入已于-20℃冷冻的甲醇800μL,振荡5 min,离心5 min,上清液按照优化的仪器工作条件分析。在Infinity Lab Poroshell 120 EC-C_(18)色谱柱(150 mm×3.0 mm, 2.7μm)上以不同体积比的含10 mmol·L^(-1)甲酸铵的0.1%(体积分数,下同)甲酸溶液和乙腈的混合溶液梯度洗脱分离米酵菌酸,以双喷射流电喷雾离子源负离子模式电离,以全离子采集一级质谱(MS1-Allions)模式定性鉴别,以基质匹配工作曲线法定量。结果显示,米酵菌酸的质量浓度在45~450μg·L^(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为3.2μg·L^(-1)。对空白全血样品进行3个浓度水平的加标回收试验,回收率为82.6%~90.1%,测定值的相对标准偏差(n=6)为4.5%~5.6%。方法应用于疑似中毒患者全血样品的分析,检出了米酵菌酸(检出量为2 225μg·L^(-1))。 展开更多
关键词 超高效液相色谱-四极杆飞行时间质谱法 米酵菌酸 全血 中毒患者
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电感耦合等离子体质谱法同时快速测定血液中15种元素的研究
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作者 张鑫 张瑛 +3 位作者 李娜 郑敏 吴虹 孙湛 《中国卫生标准管理》 2023年第14期159-164,共6页
目的建立人体血液中15种金属元素的电感耦合等离子体质谱(inductively coupled plasma mass spectrometry,ICPMS)同时快速测定的方法,为快速、准确地测定全血中金属元素提供技术支持。方法选取2022年2—6月济南市健康人群体检血液样本... 目的建立人体血液中15种金属元素的电感耦合等离子体质谱(inductively coupled plasma mass spectrometry,ICPMS)同时快速测定的方法,为快速、准确地测定全血中金属元素提供技术支持。方法选取2022年2—6月济南市健康人群体检血液样本经稀释剂稀释,离心后上机,采用碰撞反应池(kinetic energy discrimination,KED)模式同时测定全血中15种元素。结果15种元素在测定范围内具有良好的线性,相关系数均>0.999;方法检出限为0.05~0.40μg/L;平均回收率为87%~118%;相对标准偏差(relative standard deviation,RSD)为0.8%~4.2%;与全血标准物质检测结果吻合。结论本方法能够快速、准确地测定全血中15种元素,节省了分析时间,对环境友好,适用于批量全血样本中多元素的分析检测工作。 展开更多
关键词 全血 元素 电感耦合等离子体质谱仪 碰撞反应池模式 稀释剂 质谱干扰
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在线固相萃取-超高效液相色谱-串联质谱法同时测定血液样品中12种卡西酮类毒品
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作者 孙立敏 王松才 +3 位作者 林贤文 朱焕慧 刘悦 谭莉 《中国司法鉴定》 2023年第2期55-60,共6页
目的建立一种同时测定血液样品中12种卡西酮类毒品的在线固相萃取-超高效液相色谱-串联质谱法。方法血液样品用乙腈沉淀蛋白,经离心、稀释、过滤后上样,采用PLRP-S在线固相萃取柱(2.1 mm×12.5 mm,15~20μm)富集纯化,Poroshell 120 ... 目的建立一种同时测定血液样品中12种卡西酮类毒品的在线固相萃取-超高效液相色谱-串联质谱法。方法血液样品用乙腈沉淀蛋白,经离心、稀释、过滤后上样,采用PLRP-S在线固相萃取柱(2.1 mm×12.5 mm,15~20μm)富集纯化,Poroshell 120 EC-C_(18)色谱柱(3.0 mm×150 mm,2.7μm)进行分离,在线固相萃取柱以乙腈-5%(体积分数)甲醇作为流动相进行流速1.0 mL/min的梯度洗脱,色谱柱以5 mmol/L乙酸铵缓冲液[含0.1%(体积分数)甲酸]-乙腈作为流动相进行流速0.4 mL/min的梯度洗脱。离子源为电喷雾离子源,采用多反应监测模式进行测定。结果12种卡西酮类毒品线性关系良好,相关系数均大于0.998,方法检出限为0.1~0.5 ng/mL,定量限为0.3~1.5 ng/mL。12种卡西酮类毒品在3个不同质量浓度条件下的回收率为70.9%~108%,日内精密度和日间精密度分别为1.5%~8.9%、5.1%~44.5%(n=6)。结论该方法操作简单方便、样品需求量少、灵敏度高、检出限低,可用于血液样品中卡西酮类毒品的测定。 展开更多
关键词 在线固相萃取 超高效液相色谱-串联质谱法 卡西酮 血液样品 毒物分析
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超高效液相色谱-四极杆/静电场轨道阱高分辨质谱测定血液和肝脏中12种拟除虫菊酯类农药 被引量:1
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作者 张鹤耀 国菲 +1 位作者 贾振军 李鹏 《分析测试学报》 CAS CSCD 北大核心 2023年第4期439-446,共8页
建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-QE-Orbitrap HRMS)测定血液和肝脏中12种拟除虫菊酯类农药的分析方法。血液和肝脏样品经乙腈沉淀蛋白后,采用Hypersil GOLD VAN⁃QUISH色谱柱(1.9μm,2.1 mm×100 mm),以5 ... 建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-QE-Orbitrap HRMS)测定血液和肝脏中12种拟除虫菊酯类农药的分析方法。血液和肝脏样品经乙腈沉淀蛋白后,采用Hypersil GOLD VAN⁃QUISH色谱柱(1.9μm,2.1 mm×100 mm),以5 mmol/L乙酸铵溶液(含0.1%甲酸)和甲醇作为流动相进行梯度洗脱分离,采用全扫描及自动触发二级质谱(Full MS/dd-MS2)进行检测。结果显示:12种拟除虫菊酯类农药在各自线性范围内线性良好(r2≥0.9904),血液和肝脏中的检出限分别为1~18 ng/mL和1~18 ng/g,定量下限分别为2~20 ng/mL和2~20 ng/g,基质效应为82.3%~117%,回收率为74.1%~120%,日内精密度(In⁃tra-RSD)≤11%,日间精密度(Inter-RSD)≤12%。该方法满足公安机关办理实际案件要求,适用于血液和肝脏样本中拟除虫菊酯类农药的检验鉴定。 展开更多
关键词 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-QE-Orbitrap HRMS) 拟除虫菊酯 血液 肝脏 检测
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