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1.
同位素稀释液相色谱串联质谱法测定血清总胆固醇   总被引:5,自引:1,他引:4  
目的建立同位素稀释液相色谱串联质谱(LC/MS/MS)测定血清总胆固醇的方法。方法血清样品中加入[3,4-^13 C2]-胆固醇作内标,用氢氧化钠水解血清胆固醇酯为胆固醇,用三氧化铬—硫酸氧化胆固醇为胆甾-4-烯-3,6-二酮,用LC/MS/MS分析胆固醇氧化产物,采用大气压化学电离源,用多反应监测(MRM)模式和选择离子监测(SIR)模式检测,用修正标准曲线法对血清样品进行定量。结果两种检测模式的峰面积比与胆固醇浓度的线性相关系数均大于0.9999。MRM模式测定血清总胆固醇的平均批内变异系数(CV)为0.95%(范围0.92%~0.99%),平均总CV为0.86%(0.82%~0.89%);SIR模式平均批内CV为0.64%(0.54%~0.77%),平均总CV为0.69%(0.62%~0.81%)。测定国际或国家标准物质结果与靶值的平均偏差在MRM模式下为0.23%(0.14%~1.00%),SIR模式为0.24%(0.07%~1.27%)。结论成功建立了LC/MS/MS测定血清总胆固醇的方法,方法特异、精密、简便,可望用作血清胆固醇测定的参考方法。  相似文献   

2.
【目的】建立人血浆中丙泊酚浓度的高效液相色谱串联质谱法(HPLC—MS/MS)测定方法,以评价其效果。【方法】采用LC—MS/MS法测定丙泊酚的浓度,色谱柱为Zorbax Eclipse XDB-C18(50mm×4.6mm,5μm),流动相为甲醇及0.1%氨水溶液;流速0.4mL/min;电喷雾离子化电离源(ESI),质谱采用MRM模式,以负离子检测,检测离子为丙泊酚m/z177.2→m/z161.4、麝香草酚m/Z147.2→m/z106.7。20名健康志愿者静脉注射丙泊酚2mg/kg后,按预定时间点抽取动脉血进行血浆药物浓度的检测。【结果】丙泊酚血药浓度在线性范围分别为0.012~12.06μg/mI。范围内线性关系良好(r=0.9993),定量下限为0.012μg/mL;低、中、高3个浓度的日内及日间相对精密度(RSD)〈15%;平均提取回收率86.7%,RSDl.87%。【结论】本方法特异性强、灵敏、高效、精密度及准确度好,适用于人体血浆中丙泊酚的检测。  相似文献   

3.
目的建立除草剂2,4-D丁酯的气相色谱-质谱(GC/MS)检测方法,用于临床中毒患者的检测。方法以乙酸乙酯提取血液中2,4D丁酯,采用GC/MS检测。定性采用全扫描法(SCAN),定量采用选择离子法(SIM),离子选择m/z175、185、276。结果2,4-D丁酯在10~1500ng/ml成线性,方程为Y=10.565X-1203.5,R=0.9941,标加1000ng/ml浓度的2,4-D丁酯于血液,平均回收率为94.6%,RSD=7.1%;2,4-D丁酯最低检出浓度为3ng/ml(S1M),信噪比S/N=3;日内精密度RSD为4.1%,日间精密度RSD为5.8%。结论所建方法灵敏、快速、线性范围好,可用于2,4-D丁酯中毒患者的检测。  相似文献   

4.
血清尿素同位素稀释气相色谱质谱法的建立和研究   总被引:2,自引:1,他引:1  
目的 建立一种基于同位素稀释/气相色谱/质谱技术(isotope dilution/gas chromatography/mass spectrometry,ID/GC/MS)的血清尿素候选参考方法.方法 以[13C,15N2]尿素为内标,用无水乙醇沉淀、去除血清中的蛋白类物质,依次使用丙二醛-二甲基缩醛和N-甲基-(三甲基硅烷基)-三氟乙酰胺(MSTFA)将尿素衍生成为三甲基硅烷氧基嘧啶,用气相色谱/质谱(GC/MS)分析衍生产物,以包括法定量.结果 血清尿素测定的批内、批间和总变异系数的平均值分别为0.38%(范围0.12%~0.47%)、0.62%(范围0.49%~0.87%)和0.73%(范围0.51%~0.93%),回收率范围为99.37%~100.95%,分析美国国家标准和技术研究院(NIST)2个水平的血清标准物质SRM 909b,测定结果与靶值的偏差小于0.2%.结论 建立了ID/GC/MS技术测定血清尿素的方法,方法准确、精密、简便,可望作为血清尿素测定的参考方法.  相似文献   

5.
目的方法利用液体芯片一飞行质谱技术进行血清中胶质瘤疾病相关蛋白质的筛选。结果将78例胶质瘤患者和68例正常对照者血清样本各随机分为模型建立组和模型验证组;应用液体芯片.飞行质谱技术测定模型建立组样本,进行了差异蛋白的筛选和诊断模型的建立;然后用模型验证组样本进行了差异蛋白和模型的验证;并对其中的蛋白质进行鉴定。经模型建立组胶质瘤患者与正常对照者的血清蛋白质图谱比较,得到差异蛋白17个并建立了诊断模型,建模蛋白质为l460(m/z)、l612(m/z)、l776(m/z)、l862(m/z)、l941(m/z)、3952(m/z)、4052(m/z)。模型敏感性为85%,特异性为9r7.06%。其中差异蛋白质l460(m/z)、1612(m/z)、2551(m/z)为肿瘤高表达,差异蛋白l941(m/z)为肿瘤低表达,经鉴定蛋白质l941(m/z)为高分子量激肽原。结论利用液体芯片一飞行质谱技术进行血清中胶质瘤疾病相关蛋白质的研究,得到了差异蛋白和诊断模型,为临床胶质瘤的诊断提供了新的思路;差异蛋白质的鉴定结果可能为胶质瘤的治疗提供有价值的途径。  相似文献   

6.
[目的]为了发展毒鼠强的检测方法。[方法]样品经过前处理后,使用气相色谱-质谱(GC—MS)法进行测定。使用气相色谱-质谱(GC—MS)法进行毒鼠强的定性测定,并且从质谱的全扫描方式(50—400)和选择离子扫描方式(212、240)的比较来研究GC—MS上如何准确地进行定性和定量,如何提高灵敏度。[结果]毒鼠强保留时间10.62min,特征离子峰为240(分子离子峰)、212(脱N—CH2碎片离子峰)。毒鼠强在不同样品中的回收率分别为59.8%~91.2%。[结论]选择离子扫描方式去除了毒鼠强组分峰附近大部分的杂质峰,消除了试剂和样品中其他组分对毒鼠强检测的干扰,大大提高了灵敏度,非常适合于定量分析。  相似文献   

7.
目的建立测定人血浆中双氢可待因浓度的高效液相色谱一串联质谱分析方法。方法血浆样品用甲醇沉淀蛋白后,选用安捷伦色谱柱XDB.C18,2.1×50mm,5μm梯度洗脱。流动相A为0.1%甲酸10mM甲酸铵水溶液,流动相B为0.1%甲酸甲醇。流动性梯度为0min(B5%)→1min(B5%)→1.3(B65%)→2.4min(B65%)→2.5min(B5%)→3.5min(B5%)。流速0.6mL/min,柱温30℃,自动进样器温度4cC,进样量10止。选用岛津LC-20A高效液相色谱系统和串联APl4000Qtrap型三重四极杆质谱仪,ESI源正离子MRM扫描,Is电压5500V,CAD气Medium,CUR气40psi,Gasl:35psi,Gas2:40psi,源温度550℃,EP电压10V,CXP电压9V。双氢可待因:m/z302.1—199.1,DP电压:105V,CE电压:47V。右美沙芬(内标):m/z271.3→170.1,DP电压100V,CE电压54V。结果该方法测定血浆中二氢可待因的线性范围为2~1000ng/mL(r〉0.99),定量下限为2ng/mL,准确度均在85%~115%,批内和批间精密度也均〈15%。稳定性试验中,血浆样品及血浆经处理后样品中的双氢可待因在方法学要求的各种贮存条件下均比较稳定。结论该方法简单、快速、灵敏、专属性强、重现性好,适用于检测人血浆中双氢可待因浓度的研究。  相似文献   

8.
SELDI-TOF-MS技术筛选鼻咽癌患者血清标志蛋白   总被引:1,自引:1,他引:0  
目的应用表面增强激光解吸电离飞行时间质谱(SELDI—TOF—MS)技术筛选鼻咽癌(NPC)患者血清中的标志蛋白。方法用CiphergenBiosystem公司生产的PBSⅡ/C型蛋白质指纹图谱仪和GoldChip(金芯片)蛋白芯片检测98例鼻咽癌患者和30例正常人血清的蛋白指纹图谱,采用Biomaker Wizard 3.1软件分析两组的蛋白表达情况筛选差异表达蛋白。结果两组均检出较多蛋白峰,并且有表达明显的蛋白峰(P〈0.01),在鼻咽癌患者中,低表达的有1个(即m/z为5026Da),高表达的有4个(即m/z为5934Da,5352Da,6655Da,6675Da)。结论用SELDI—TOF—MS蛋白质芯片技术筛选NPC患者血清中特异性蛋白标志物对鼻咽癌的早期诊断具有较大价值。  相似文献   

9.
血清胆汁酸LC-MS/MS测定及在老年人血清检测中的应用   总被引:4,自引:0,他引:4  
目的:建立稳定、有效的血清中所有胆汁酸的液相色谱-串联质谱(LC-MS/MS)测定方法,分析老年人血清胆汁酸谱的特征。方法:建立血清胆汁酸LC-MS/MS定量检测方法,并对方法的灵敏度、精密度、回收率、线性范围等性能指标进行评价;利用该检测方法对10例老年人和15例儿童的空腹血清中所有胆汁酸进行定量检测,分析老年组血清胆汁酸组成特征。结果:该检测体系中,血清中15种胆汁酸和内标在10分钟内完成定量检测,最低检测极限为2~4ng/ml,浓度在3.9~3000ng/ml范围内线性良好,相对回收率为91.95~108.25%,偏移系数为1.71%~10.83%,日内变异度为0.68%~7.05%,日间变异度为2.04%~11.05%;与儿童组相比,老年组血清中胆汁酸总量、疏水性胆汁酸的含量百分较高。结论:所建立的胆汁酸LC-MS/MS检测方法稳定可靠,能满足临床定量检测要求;老年人体内血清胆汁酸谱可能促进胆石症的发生。  相似文献   

10.
目的优化高效液相色谱串联质谱法(LC-MS/MS)测定血清游离雌三醇(uE3)的前处理方法。方法以活性炭吸附血清为研究基质,通过加入已知量的雌三醇(E3)标准品及E3-2-3-4-13 C3内标,在LC-20AD XR高效液相色谱系统和API 5500串联四级杆质谱仪上对E3检测的色谱条件、质谱条件及萃取条件等进行优化。结果色谱条件:选用菲罗门Knietex色谱柱(100.0mm×2.1mm,2.6μm);有机相为甲醇,水相为0.1mmol/L氟化铵水溶液,8min梯度洗脱。质谱条件:选用电喷雾(ESI)负离子模式和多反应监测(MRM)模式分析,选择质荷比(m/z)287→m/z 145作为E3的定量离子对,m/z 287→m/z 171作为定性监测离子对;选择m/z 290→m/z 148作为内标的定量离子对,m/z 290→m/z 174作为定性监测的离子对。萃取条件:萃取剂为正己烷/乙酸乙酯(50/50,v/v),样品与萃取剂的比例为1∶2,萃取率可达85.71%。结论 E3检测的色谱条件、质谱条件、萃取条件已得到全面优化,为后续建立LC-MS/MS测定人血中uE3的参考方法打下良好基础。  相似文献   

11.
Objective: To identify patterns of nonfatal and fatal penetrating trauma among children and adults in New Mexico using ED and medical examiner data.
Methods: The authors retrospectively sampled in 5-year intervals all victims of penetrating trauma who presented to either the state Level-1 trauma center or the state medical examiner from a 16-year period (1978–1993). Rates of nonfatal and fatal firearm and stabbing injury were compared for children and adults.
Results: Rates of nonfatal injury were similar (firearm, 34.3 per 100,000 person-years; stabbing, 35.1). However, rates of fatal injury were significantly different (firearm, 21.9; stabbing, 2.7; relative risk: 8.2; 95% confidence interval: 5.4, 12.5). From 1978 to 1993, nonfatal injury rates increased for children (p = 0.0043) and adults (p < 0.0001), while fatal penetrating injury remained constant. The increase in nonfatal injury in children resulted from increased firearm injury rates. In adults, both stabbing and firearm nonfatal injury rates increased.
Conclusions: Nonfatal injury data suggest that nonfatal violence has increased; fatal injury data suggest that violent death rates have remained constant. Injury patterns vary by age, mechanism of trauma, and data source. These results suggest that ED and medical examiner data differ and that both are needed to guide injury prevention programs.  相似文献   

12.
Three supplementary perspectives are presented arguing that interprofessional collaboration is both necessary and desirable. Nonetheless, there are often too many serious intra-professional barriers and obstacles to interprofessional collaboration to make it successful. Some of these barriers, it is argued and illustrated, are found in the multiple ways in which professional identity is tacitly acquired and embodied in the practitioners' habitual, everyday practice. The paper then explores ways in which reflection, especially Second order reflection, can help to elucidate and overcome these obstacles, as well as increasing professional adaptability and competence.  相似文献   

13.
This is a new method for the determination of creatine kinase isoenzyme MB activity in serum. The method uses direct activity measurement of creatine kinase B subunit activity after blocking of CK-M subunit activity by inhibiting antibodies. The test takes no longer than 15 min. The method yields an intra-serial C.V. of 2.0-12.9%, and a C.V. from day to day of 5.5%. The detection limit is 3.4 U/l creatine kinase MB. In the 95 cases with proven myocardial infarction several types of creatine kinase MB activity kinetics could be determined. The percentage of creatine kinase MB of peak CK-total is 6-25%, with a mean of 11.1%. The amount of creatine kinase MB with respect to total CK activity after reinfarction is higher than the amount after initial infarction.  相似文献   

14.
Ranganath C  Heller AS  Wilding EL 《NeuroImage》2007,35(4):1663-1673
Although substantial evidence suggests that the prefrontal cortex (PFC) implements processes that are critical for accurate episodic memory judgments, the specific roles of different PFC subregions remain unclear. Here, we used event-related functional magnetic resonance imaging to distinguish between prefrontal activity related to operations that (1) influence processing of retrieval cues based on current task demands, or (2) are involved in monitoring the outputs of retrieval. Fourteen participants studied auditory words spoken by a male or female speaker and completed memory tests in which the stimuli were unstudied foil words and studied words spoken by either the same speaker at study, or the alternate speaker. On "general" test trials, participants were to determine whether each word was studied, regardless of the voice of the speaker, whereas on "specific" test trials, participants were to additionally distinguish between studied words that were spoken in the same voice or a different voice at study. Thus, on specific test trials, participants were explicitly required to attend to voice information in order to evaluate each test item. Anterior (right BA 10), dorsolateral prefrontal (right BA 46), and inferior frontal (bilateral BA 47/12) regions were more active during specific than during general trials. Activation in anterior and dorsolateral PFC was enhanced during specific test trials even in response to unstudied items, suggesting that activation in these regions was related to the differential processing of retrieval cues in the two tasks. In contrast, differences between specific and general test trials in inferior frontal regions (bilateral BA 47/12) were seen only for studied items, suggesting a role for these regions in post-retrieval monitoring processes. Results from this study are consistent with the idea that different PFC subregions implement distinct, but complementary processes that collectively support accurate episodic memory judgments.  相似文献   

15.
ABSTRACT

The Cochrane Library of Systematic Reviews is published quarterly as a DVD and monthly online. The January 2011 issue (first quarterly DVD for 2011) contains 4515 complete reviews, 1985 protocols for reviews in production, and 13,521 one-page summaries of systematic reviews published in the general medical literature. In addition, there are citations of 641,000 randomized controlled trials, and 14,018 cited papers in the Cochrane methodology register. The health technology assessment database contains over 9300 citations. One hundred and seven new reviews have been published in the last 3 months, of which five have potential relevance for practitioners in pain and palliative medicine.  相似文献   

16.
目的 探讨手转胎头术失败的原因与分娩结局.方法 选择2008年1月至2010年12月于我院住院分娩的持续性枕横位、枕后位产妇198例,根据行手转胎头术后结果分为成功组126例、失败组72例.比较两组分娩结局,对比分析失败原因.结果 失败组胎儿体质量≥3500 g的发生率[76.4%(55/72)]明显高于成功组[31.7%(40/126)],差异有统计学意义(x2=30.177,P=0.001)、失败组宫缩乏力发生率[58.3%(42/72)]高于成功组[38.1% (48/126)],差异有统计学意义(x2=7.569,P=0.006)、失败组骨盆临界或轻度狭窄发生率[38.9% (28/72)]高于成功组[23.8%(30/126)],差异有统计学意义(x2 =5.030,P=0.002)、失败组手转胎头时机不当(宫口开大<6 cm、胎头位于坐骨棘上及宫口开大8~10 cm、胎头位于坐骨棘下≥2 cm)发生率[61.1%(44/72)]高于成功组[38.9%(49/126)],差异有统计学意义(x2=9.084,P=0.003).失败组母儿并发症(产后出血、产褥病率、胎儿窘迫、新生儿窒息)发生率高于成功组(x2 =9.586,P=0.002、x2=9.334,P=0.002、x2=5.910,P=0.015、x2=5.240,P=0.022)、失败组剖宫产发生率[72.2%(52/72)]明显高于成功组[34.1 %(43/126),x2=26.641,P=0.001)].结论 手转胎头术能使难产变顺产,降低剖宫产率,减少母儿并发症,但须积极预防、处理导致手转胎头术失败的原因,对矫正失败后继续矫正及试产应慎重.  相似文献   

17.
The Department of Veterans Affairs (VA) in the USA operates a network of 172 medical centres which all utilize a hospital information system (HIS) which has been developed and is currently maintained by the VA. During the past several years, an image management and communication module has been developed, installed and clinically utilized at the Washington DC and Maryland VA Medical Centres. This image management and communication system, referred to as the decentralized hospital computer program (DHCP) imaging system, is fully integrated with a commercial picture archiving and communication system (PACS). The system is utilized to capture, archive, and display all images generated within the hospital including radiology, nuclear medicine, pathology, endoscopy, bronchoscopy, and dermatology, intraoperative photographs, ECG data, and a limited number of paper documents. The ultimate goal of the project is to have all patient text and image data available at any clinical workstation to any authorized user anywhere within the network of medical centres. Clinical requirements for an imaging workstation include ease of use, rapid and reliable access to the complete set of patient information, and images which are of acceptable quality to meet the requirements of the user and the subspecialty. Patient confidentiality and data security must be safeguarded at all times. Integration of the images with the remainder of the patient's database was found to be critical to the success of the project. The experience at the Washington and Maryland facilities suggests that an imaging system that is successfully integrated with a hospital information system can provide substantial clinical and economic benefits both within and among medical centres. Clinical acceptance and utilization of the system has been excellent, particularly in diagnostic radiology where DHCP Imaging has been interfaced to a commercial PAC system. Based upon this initial experience, the VA has begun to deploy the system throughout its large network of medical centres.  相似文献   

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目的 探讨俯卧位通气对高海拔地区肺复张术(RM)治疗无效急性呼吸窘迫综合征(ARDS)患者的治疗作用.方法 从海拔2260m的地区医院筛选RM治疗无效的41例ARDS患者[平均氧合指数( PaO2/FiO2)较RM前升高<20%视为RM无效],依不同病因分为肺内源性ARDS组(ARDSp组)和肺外源性ARDS组(ARDSexp组),每组再按信封法随机分为俯卧位组和仰卧位组,即ARDSp俯卧位组(11例)、ARDSp仰卧位组(9例)、ARDSexp俯卧位组(10例)、ARDSexp仰卧位组(11例).在通气前及通气1、2、3、4h监测动脉血氧分压( PaO2)、PaO2/FiO2、静态顺应性(Cst)、气道阻力(Raw)的变化.结果 通气lh时,ARDSexp俯卧位组PaO2/FiO2( mm Hg,l mm Hg=0.133 kPa)即较通气前显著升高(157.4±40.6比129.3±48.7,P<0.05),并随通气时间延长呈持续增高趋势,4h达峰值(219.1 ±41.1);且ARDSexp俯卧位组通气3h内PaO2/FiO2较其他3组显著增高,另3组间则差异无统计学意义.ARDSp俯卧位组、ARDSexp俯卧位组通气4h时PaO2/FiO2均较相应仰卧位组显著增高(208.8±39.7比127.4±47.1,219.1±41.1比124.9±50.8,均P<0.05).4组通气前后Cst无显著改变,各组间差异也无统计学意义.ARDSp俯卧位组通气4h时Raw(cmH2O·L-1·s-1)较通气前显著降低(6.8±1.7比10.7±1.8,P<0.05),且明显低于其他3组;其他3组各时间点Raw组内及组间比较差异均无统计学意义.结论 俯卧位通气作为ARDS机械通气重要策略之一,可以改善RM无效高原ARDS患者的氧合,为抢救患者赢得宝贵的时间.  相似文献   

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