GC—MS法鉴定银柴胡挥发油的化学成分

目的 研究银柴胡的挥发油化学成分。方法 采用气相色谱-质谱联用仪(GC-MS)对银柴胡的挥发油化学成分进行了分析鉴定。结果 从分离出的20多个峰中鉴定出17个化学成分。结论 银柴胡挥发油的主要化学成分为2-甲基-5-异丙烯基-2，5-己二烯-1-乙酸酯，去乙酰基蛇形毒素和14-甲基十五烷酸甲酯等成分。     

不同来源板蓝根药材乙酸乙酯提取物HPLC指纹图谱分析

目的建立不同来源板蓝根药材乙酸乙酯提取物特征指纹图谱。方法采用反相高效液相色谱法，ODS-C18色谱柱（250mm×4．6mm，5μm．），流动相为甲醇-0．2％磷酸水溶液系统，线性梯度洗脱，检测波长230nm，进样量为10μl。实验测定了10批药材并记录了指纹图谱，不同样品之间的相似度采用国家药典委员会开发的中药指纹图谱相似度评价系统（2004A）计算。结果建立了板蓝根药材乙酸乙酯提取物HPLC指纹图谱，以峰形较好、峰面积较高的3号峰为参照峰，确立了板蓝根药材乙酸乙酯提取物指纹图谱的14个特征共有峰，但特征峰的相对含量差异较大，导致指纹概貌差异。结论所建立的HPLC指纹图谱有很好的精密度、重现性和稳定性，为深入研究板蓝根的质量标准提供了实验基础。     

GC-MS法测定干姜超临界CO2萃取物的化学成分及其姜酚类成分的追踪

目的 分析干姜超临界CO2萃取物的化学成分,并追踪萃取物中的姜酚类成分.方法 采用超临界CO2萃取干姜药材,用气相色谱-质谱联用技术分析其成分,6-姜酚和1O-姜酚直接进样分析,将姜酚图谱与萃取物图谱进行对比分析.结果 从干姜超临界CO2萃取物中鉴定了52种成分.在6-姜酚和10-姜酚的气相色谱-质谱分析过程中追踪到两...     

猕猴血浆中SARS冠状病毒主蛋白酶肽类抑制剂N3的测定

目的建立测定猕猴血浆中N3的LC-MS/MS法。方法以ffiOBasiCC18（100mm×2.1 mm,5μm）色谱柱为 分析柱,流动相为乙腈-水（含0.2%甲酸）（55：45, F：F）,采用电喷雾离子源（ESI）,正离子扫描方式,选择离子反应监测 （SRM）模式检测,用于定量分析的离子反应为m/z681.3-402.3。结果血浆中的N3用乙腈沉淀蛋白后,样品经LC-MS/MS 系统进行检测。在优化后的样品预处理、色谱及质谱条件下,LC-MS/MS法检测猕猴血浆中的N3,线性范围为20 -2500 μg·L^-1,准确度RE范围为-12.9% -2. 9 %,日内、日间精密度的RSD分别小于7.5% （ n =6）和7.8% （ n =18）;低、中、高 3个浓度（50、1000和2000μg·L^-1）犯质控样品的提取回收率分别为75.5 %、77.3 %和79.6 %。结论结果表明,该方法 具有灵敏、准确、快速等优点,适用于N3在猕猴体内的药代动力学研究。     

小儿鼻炎片的质量标准研究

目的建立小儿鼻炎片的质量标准。方法采用薄层色谱法对小儿鼻炎片中的白芷、升麻、和防风等药材进行了薄层色谱鉴别;采用高效液相色谱法测定了君药藁本药材中阿魏酸的含量,色谱柱为Agilent ZORBAX SB-C18（250mm×4.6mm,5μm）分析柱;流动相：甲醇-0.1%磷酸溶液（25∶75）;流速：1.0mL/min;检测波长：320nm;柱温：40℃。结果薄层色谱法可鉴别出该制剂中的白芷、升麻、和防风。阿魏酸在0.028 8～5.67μg范围内有良好的线性关系,r=0.999 5,平均回收率为100.6%,RSD为1.54%（n=6）。结论该方法准确、灵敏、重复性好,能有效地控制小儿鼻炎片的质量。     

青芹籽低极性部位化学成分GC-MS分析

目的 研究青芹籽低极性部位的主要化学成分。方法 采用GC—MS法对青芹籽低极性部位进行分析。结果 共检出了27个化学成分，主要化学成分与文献报道的芹菜籽挥发油化学成分大致相同，其中主要活性成分正丁基苯酞和瑟丹内酯含量较高。结论青芹籽低极性部位主要成分为瑟丹内酯（约70．66％）和正丁基苯酞（13．45％），并含有4（14），11-桉叶二烯（3．49％）、油酸（2．11％）、棕榈酸（1．49％）等化学成分。     

茂汶黄芪化学成分研究

目的对茂汶黄芪（Astragalus maowenensis Hsiao．）根的化学成分进行研究，分离并鉴定化合物。方法采用现代层析分离技术进行化学成分的分离，运用光谱方法确定所分离化合物的结构。结果从中分离得到5个化合物，分别为毛蕊异黄酮-7-O-β-D-吡喃葡萄糖苷（Ⅰ），乙酰黄芪皂苷（Ⅱ），黄芪皂苷Ⅰ（Ⅲ），黄芪皂苷Ⅱ（Ⅳ），黄芪皂苷Ⅳ（Ⅴ）。结论以上化合物均为首次从该植物中分得。     

HPLC测定藏药螃蟹甲中8-乙酰氧基山栀子苷甲酯的含量

目的建立藏药螃蟹甲中8-乙酰氧基山栀子苷甲酯的HPLC测定方法,为进一步控制螃蟹甲药材及其制剂的质量提供参考依据。方法色谱柱为SymmetryC18（4．6mm×150mm,5μm）,流动相：乙腈-水（6：94）,HAe调pH=4．50,流速0．8mL／min,柱温20℃,检测波长234nm。结果8．乙酰氧基山栀子苷甲酯浓度在0．787～14．76μg·mL^-1范围内与峰面积积分值线性关系良好（r=0．9999）;加样回收率为99．21％（RSO=1．68％）。螃蟹甲药材中8-乙酰氧基山栀子苷甲酯平均含量为（0．62±0．19）mg·g^-1。结论本方法简便、准确、专属性强,可用于螃蟹甲药材中8-乙酰氧基山栀子苷甲酯的含量测定。     

络石藤黄酮类化学成分研究

目的对络石藤中的黄酮类化学成分进行分离鉴定。方法采用硅胶，Sephadex LH-20等柱色谱方法进行分离，光谱和化学方法进行结构鉴定。结果分离鉴定了5个黄酮，分别是：芹菜素（Ⅰ），4′，5，7-三羟基-3′-甲氧基黄酮（Ⅱ），槲皮苷（Ⅲ），大豆苷（Ⅳ），芹菜素-7-O-β-D-葡萄糖苷（V）。结论化合物Ⅱ，Ⅲ和Ⅳ为从络石属植物中首次分离。     

亲水色谱-质谱联用（HILIC-MS）定量测定大鼠血浆中美金刚浓度及药代动力学研究

目的建立灵敏、可靠的亲水色谱-质谱联用（HILIC-MS）方法测定大鼠血浆中美金刚的浓度。方法血浆样品前处理采用蛋白沉淀,用HILIC-MS法测定。通过电喷雾电离源以选择离子监测（SIM）方式进行正离子检测,用于定量分析的离子分别为m/z 180（美金刚）和m/z 285（内标Ro 64-0802）。色谱分离采用Amide-80柱（100 mm×4.6 mm,5μm）,以乙腈-水-甲酸（70∶30∶0.1,v/v/v,0.35 ml/min）为流动相。结果美金刚的线性范围为2～500 ng/ml,相关系数r2为0.99882,定量下限为2 ng/ml,批内、批间精密度在3.9%和5.6%以内,准确度控制在84.9%～111.2%。结论本方法通过HILIC技术,使美金刚保留时间增加,基质抑制降低并使检测灵敏度提高。该方法成功应用于大鼠血浆测定研究中。     

GC-MS结合主成分分析法对不同产地旱莲草药材挥发性成分的比较分析

目的运用GC-MS对不同产地的4种旱莲草的挥发性成分进行比较分析。方法采用静态顶空技术,GC-MS技术,结合NIST05数据库对旱莲草的挥发性成分进行分析鉴定,并用主成分分析,对结果进行验证。结果共鉴别出旱莲草中34个挥发性成分,含量较高的成分为十五烷和十七烷。结论不同产地的旱莲草在成分和含量上存在一定差异。     

多层螺旋CT血管成像在椎基底动脉延长扩张症中的诊断价值

目的 探讨多层螺旋CT三维血管成像(MS 3D-CTA)在椎基底动脉延长扩张症(VBD)中的诊断价值.方法 对10例VBD患者(病例组)的MS 3D-CTA资料进行回顾性分析.使用GELightspeed pro 16层螺旋CT扣描仪获得原始图像,对所有患者均采用容积重组(VR)和最大密度投影(MIP)技术对图像进行三维重组.选择20名同一时期因怀疑脑血管病变而行MS 3D-CTA检查,脑血管正常者作为对照组,病例组和对照组间比较采用Wilcoxon符号秩和检验.结果 10例VBD病例组中,单纯型4例,骑跨型6例.病例组基底动脉(BA)的长度(B1)、偏移程度(Bc)、高度(Bh)和椎动脉(VA)的长度(V1)、偏移程度(Vc)以及两者的直径(Bw/Vw)分别为30.20、7.10、8.80、23.00、5.95、5.05 mm,与对照组的B1 25.60 mm、Bc 1.20 mm、Bh 1.90 mm、V1 17.55 mm、Vc 2.05 mm、B/Vw3.05 mm分别比较,差异均存在统计学意义(P值均＜0.01).结论 VBD临床表现复杂多样,MS3D-CTA是一种有效的评价椎基底动脉延长扩张症的检查技术.     

液相色谱串接质谱测定马饲料中的三种生物碱

本文建立了采用高效液相色谱串接质谱(LC-MS/MS)同时快速筛查和定量测定马复合饲料中三种天然痕量生物碱(吗啡、可待因、罂粟碱)的方法。样品经充分粉碎后用1 mmol/L HClO4溶液提取,并通过混合型固相萃取进行净化。采用ZORBAX Eclipse Plus-C18(150 mmL×2.1mm ID,3.5μm)色谱柱以含0.4%甲酸的水溶液和乙腈作为流动相进行梯度洗脱,正离子多反应监测(MRM)模式下进行检测。吗啡的检出限为0.50 ng/g,定量限为1.0 ng/g;可待因的检出限为0.75 ng/g,定量限为1.5 ng/g;罂粟碱的检出限为0.20 ng/g,定量限为0.50 ng/g。三种药物空白饲料高、中、低添加浓度水平下的回收率在77.4~97.8%之间,日内、日间精密度分别不高于6.2%和7.1%,实验结果表明本方法有较好的灵敏度和精密度,可以满足马饲料中该类药物的常规检测分析。     

Quantification of tumor tissue populations by multispectral analysis.

Tumor heterogeneity complicates the quantification of a therapeutic response by MRI. To address this issue, a novel approach has been developed that combines MR diffusion imaging with multispectral (MS) analysis to quantify tumor tissue populations. K-means (KM) clustering of the apparent diffusion coefficient (ADC), T2, and proton density (M0) was employed to estimate the volumes of viable tumor tissue, necrosis, and neighboring subcutaneous adipose tissue in a human colorectal tumor xenograft mouse model. In a second set of experiments, the temporal evolution of the MS tissue classes in response to therapeutic intervention Apo2L/TRAIL and CPT-11 was observed. The multiple parameters played complementary roles in identifying the various tissues. The ADC was the dominant parameter for identifying regions of necrosis, whereas T2 identified two necrotic subpopulations, and M0 contributed to the differentiation of viable tumor from subcutaneous adipose tissue. MS viable tumor estimates (mean volume = 275 +/- 147 mm(3)) were highly correlated (r = 0.81, P < 0.01) with histological estimates (117 +/- 51 mm(3)). In the treatment study, MS viable tumor volume (at day 10) was 77 +/- 67 mm(3) for the Apo2L/TRAIL+CPT-11 group, and was significantly reduced relative to the control group (292 +/- 127 mm(3), P < 0.01). This method shows promise as a means of detecting an early therapeutic response in vivo.     

Quantitative determination of MS-induced corpus callosum atrophy in vivo using MR imaging

To quantitate the extent of corpus callosum atrophy in multiple sclerosis, midsagittal corpus callosum areas were determined in 48 controls with normal MR scans and 41 patients with definite multiple sclerosis. The mean midsagittal corpus callosum area was 601 mm2 (range 405-791), 641 mm2, and 561 mm2 for all adult controls, for adult males, and for adult females, respectively. Control values were significantly greater than the means determined for all multiple sclerosis (MS) patients (508 mm2, range 281-758), for MS men (528 mm2), or for MS women (498 mm2). The degree of corpus callosum atrophy paralleled the estimated volume of periventricular and corpus callosum high-signal lesions, suggesting a possible cause-effect relationship. The results indicate that corpus callosum atrophy occurs commonly in patients with typical clinical forms of multiple sclerosis.     

衍生化LC-MS/MS测定大鼠血浆中新型抗流感药物帕拉米韦及其在药代动力学研究中的应用

目的：建立灵敏、可靠的衍生化LC-MS/MS新方法测定大鼠血浆中帕拉米韦的浓度。方法：血浆样品前处理包括蛋白沉淀和用盐酸（10mol/L）-甲醇（10：90,体积比）为衍生化试剂的衍生化反应,测定采用LC-MS/MS。通过电喷雾电离源以选择反应监测（SRM）方式进行正离子检测,用于定量分析的离子反应分别为m/z343→284（帕拉米韦衍生物）和m/z299→152（内标Ro64-0802衍生物）。色谱分离采用ZorbaxRX-C8柱（2.1mm×150mm,5μm）,以乙腈-水-甲酸（30：70：0.1,体积比,0.2ml/min）为流动相。结果：测定帕拉米韦的线性范围为10～10000ng/ml,相关系数r2为0.9940,定量下限为10ng/ml,批内和批间RSD%分别在5.0%和7.1%以内,准确度控制在89.9%～106.1%。结论：本方法通过衍生化反应,使帕拉米韦保留时间增加,基质抑制降低并使检测灵敏度提高。该方法成功应用于帕拉米韦非临床和临床研究中。     

Paternity testing with VNTR DNA systems

Summary Paternity testing using DNA polymorphism of variable numbers of tandem repeat (VNTR) regions with restriction fragment length polymorphism (RFLP) was implemented. HinfI-digested DNA was separated by electrophoresis in agarose gels and hybridized with radiolabelled probes detecting the VNTR-systems D2S44 (YNH24), D5S43 (MS8), D7S21 (MS31), D7S22 (g3), and D12S11 (MS43a). The intra gel variability of 970 duplicate investigations on the same gel of DNA from 122 individuals showed no differences exceeding 1.25 mm between the positions of the corresponding DNA fragments. The comparison of 1,624 DNA fragments from 342 mother/child pairs showed only one difference above 1.25 mm which was interpreted as a mutation. Based on these observations, we decided to consider an intra gel difference above 1.25 mm between the non-maternal DNA fragment of the child and the nearest DNA fragment of the putative father as an exclusion in paternity testing. This matching criterion was used for the comparisons of 1,197 DNA fragment differences in 247 pairs of children and putative fathers who had not been excluded by conventional marker systems. In all of these cases, the migration differences between the DNA fragments of non-excluded men and the DNA fragments of the children were less than 1.25 mm except in 6 cases (0.5%). The man/child differences in all of 227 false trios exceeded 1.25 mm in 2 or more of the 5 VNTR systems investigated. Matching criteria for inter gel comparisons in paternity testing were established. The frequency distribution of Hinfl digested DNA fragments of the 5 VNTR systems in 650 unrelated Danes is presented and the raw data is available.     

The effect of section thickness on MR lesion detection and quantification in multiple sclerosis.

BACKGROUND AND PURPOSEThe purpose of our study was to investigate the effect of section thickness on MR detection of brain lesion volume and measurement precision in patients with multiple sclerosis (MS).METHODSEight subjects with known MS were studied on a 1.5-T MR system. We used a 3D fast fluid-attenuated inversion-recovery sequence to obtain contiguous axial brain images at section thicknesses of 5 mm, 3 mm, and 1 mm. Two sets of images were acquired at each section thickness during two sessions, between which the patient was removed from the scanner. Lesion volumes were measured at each section thickness using a semiautomated local thresholding technique.RESULTSWe found that progressive reduction in section thickness led to detection of smaller lesions, resulting in a significant (8%) increase in lesion volume on MR images as section thickness was reduced from 5 mm to 3 mm. However, despite a further increase in lesion detection at a section thickness of 1 mm, this did not result in an increase in total lesion volume. This finding indicates that the relationship between section thickness and lesion volume on MR images is not linear. Scan-rescan reproducibility was improved by reducing section thickness, at the cost of increased analysis time.CONCLUSIONThis study shows that acquisition of very thin sections increases the sensitivity and precision of MS lesion measurement. Serial studies assessing lesion changes over time are needed to define the impact of this increase on sample size requirements for MS treatment trials.     

LC－MS／MS同时测定比格犬血浆中美托拉宗和缬沙坦

目的：建立同时测定比格犬血浆中美托拉宗和缬沙坦的高效液相色谱串联质谱法。方法分析柱为Agilent Poroshell 120色谱柱（2．1 mm ×30 mm ×2．7μm）。质谱采用电喷雾离子源（ESI）,采用多反应监测（MRM）,检测离子为正离子,分别选择m／z 366．2／259、436．2／291和423．4／207作为美托拉宗、缬沙坦和内标（氯沙坦钾）的检测离子对。结果美托拉宗、缬沙坦的线性范围分别为0．5～100及5～5000 ng／ml,相关系数r2分别为0．9937和0．9939,批内精密度分别为2．09％～8．85％和2．36％～13．12％,基质效应分别为87．73％～98．62％和99．03％～137．35％,回收率分别为75．74％～81．82％和83．89％～95．64％。结论该法操作简单、准确可靠、检测灵敏度高,可用于复方美托拉宗缬沙坦速释片比格犬体内的药代动力学研究。     

Quantitative functional MR imaging of the visual cortex at 1.5 T as a function of luminance contrast in healthy volunteers and patients with multiple sclerosis

BACKGROUND AND PURPOSE: In patients with multiple sclerosis (MS), a few preliminary functional MR (fMR) imaging studies of the visual cortex reveal information about magnitude differences between healthy individuals and patients with MS at only a single luminance level. We therefore investigated whether varying luminance contrast levels can help uncover subtle changes in fMR imaging characteristics of the visual cortex in healthy volunteers and patients with MS. METHODS: Blood oxygenation level-dependent fMR imaging signal changes in the primary visual cortex were examined as a function of luminance contrast at 1.5 T in 10 healthy volunteers and nine patients with MS. Ten axial sections through the calcarine fissure were obtained with an echo-planar T2*-weighted imaging sequence (4000/54/1 [TR/TE/excitation]; field of view, 220 mm; voxel size, 1.72 x 1.72 x 5 mm). The imaging series consisted of an alternating 20-second rest epoch (black screen) with a 20-second activation epoch (flickering checkerboard) repeated six times. Each imaging series used a graded increase of eight luminance contrast levels. A paired t test between rest and activation images was used to analyze significant (P <.001) contiguous voxels in the region of interest (primary visual cortex). RESULTS: A progressive increase in fMR imaging activation across all luminance contrast levels in healthy controls and patients with MS was shown. The patients with MS had a significantly lower magnitude in the number of fMR imaging activated voxels at all luminance contrast levels (P <.001). A statistically significant increase in fMR imaging activation (activation threshold) was seen at the second luminance contrast level in controls and at the seventh level in patients with MS. CONCLUSION: Quantifiable changes in blood oxygenation level-dependent signal and a progressive increase in activated voxels within the primary visual cortex with increasing luminance contrast were demonstrated at 1.5 T in controls. The patients with MS showed a significant decrease in the number of activated voxels and an increase in activation threshold compared with healthy controls.