GC法同时测定鱼腥草注射液中4种成分的含量

目的:建立同时测定鱼腥草注射液中4-萜烯醇、α-松油醇、乙酸龙脑酯和甲基正壬酮含量的方法.方法:采用气相色谱法;色谱柱:DB-1毛细管气相色谱柱(30m×0.25 mm,0.25μm);程序升温:70℃保持5 min,以5℃·min-1上升至140℃,保持5 min,再以20℃·min-1升至250℃;进样口温度:25...     

羌活和独活药材气相色谱指纹图谱的建立及鉴别

目的为羌活和独活药材的鉴别提供科学依据。方法采用气相色谱(GC)-氢火焰离子化检测法。色谱柱:DB-1毛细管柱(30 m×0.25 mm×0.25μm);程序升温:起始柱温50℃,8℃.min-1升至85℃保持12 min,4℃.min-1升至155℃保持18 min,12℃.min-1升至250℃保持5 min;气化室温度:250℃;载气:氮气;流速:1.2 mL.min-1;进样量:1.0μL;分流比:10∶1;检测器温度:270℃。结果建立了羌活和独活药材的GC指纹图谱;对不同产地药材分别进行了相似度计算;指纹图谱和相似度计算结果显示,羌活和独活药材挥发油含量具有明显区别。结论本方法可用于羌活和独活药材的定性鉴别。     

不同产地苍艾挥发油的GC-MS指纹图谱研究

目的:建立苍艾挥发油的气相色谱-质谱(GC-MS)指纹图谱,分析苍艾挥发油的化学组成,为其质量控制提供方法和依据.方法:Agilent DB-5MS石英毛细管色谱柱(30m×0.25mm×0.25μm),柱温40℃(保持1 min),以10℃·min-1速率升至130℃(保持5 min),以8℃·min-1速率升至25...     

毛细管气相色谱法测定盐酸头孢他美酯中残留溶剂

目的 建立顶空进样和直接进样毛细管气相色谱法测定盐酸头孢他美酯中的残留溶剂. 方法 异丙醇、乙酸乙酯、丙酮测定采用顶空进样法, 色谱柱：HP INNOWAX PEG 20M毛细管柱(30.0 m×320μm, 0.25 μm), 柱温为50 ℃, 维持5 min, 以每分钟30 ℃速率升至200 ℃, 维持3 min , 二甲亚砜为溶剂; 二甲基甲酰胺测定采用直接进样法, 色谱柱为DB 624(6%氰丙基苯基 94%二甲基聚硅氧烷固定液)石英毛细管柱(30.0 m×0.53 mm,3.0 μm), 柱温为100 ℃, 维持6 min, 以每分钟30 ℃速率升至200 ℃, 维持5 min, 二甲亚砜为溶剂. 结果 被测物均能得到很好的分离, 峰面积与浓度呈良好的线性关系, 精密度和回收率良好. 结论 该法可用于盐酸头孢他美酯原料药中残留溶剂的检测.     

野菊花注射液的GC指纹图谱

目的建立野菊花注射液GC指纹图谱。方法使用DB-17弹性石英毛细管柱(30 m×0.25 mm,0.25μm)。柱温:初温80℃保持5 min,以5℃.min-1升至100℃保持10 min,5℃.min-1升至170℃保持5 min,10℃.min-1升至250℃保持3 min;载气:高纯氮气,流量,1.0 mL.min-1;分流比10∶1;氢气:40 mL.min-1;空气:400 mL.min-1;检测器:FID;检测器温度:280℃;气化室温度:280℃;进样量:1μL。结果建立了野菊花注射液的对照指纹图谱并确定了22个共有峰,各批注射液与对照指纹图谱相似度均在0.95以上。结论该方法简便、准确、重现性好,为野菊花注射液的质量控制提供了依据。     

顶空-气相色谱法测定药酒中的甲醇量

目的建立药酒中甲醇量的测定方法。方法采用顶空-气相色谱法,色谱柱为Agilent Technologies DB-WAX(30m×0.32mm×0.25μm),FID检测器;进样口温度:140℃;检测器温度220℃;载气流速:0.3 mL·min-1;梯度升温:29℃保持1min,以0.5℃·min-1速率升至31℃,保持10min,以5℃·min-1速率升至65℃,保持1 min,以50℃·min-1速率升至200℃,保持2min;时间周期:38min。结果甲醇在0.000 1~0.005mL·mL-1范围内线性关系良好,r=0.999 4,平均回收率为99.6%,RSD 2.5%(n=6)。结论该方法检测结果准确、专属性强、灵敏度高、重复性好,可用于药酒中甲醇量的控制。     

气相色谱法测定保济丸中百秋李醇的含量

目的:建立以气相色谱法测定保济丸中百秋李醇含量的方法,制定并完善保济丸的质量标准。方法:采用非极性毛细管柱AT.SE-54(15m×0.25mm×0.33μm),柱温采用程序升温:起始150℃,保持23min,以8℃·min-1速率升至230℃,保持2min,进样口温度为280℃,检测器(FID)温度为280℃,载气为氮气,流速为1.0mL·min-1。结果:百秋李醇进样量在0.12～0.36μg范围内线性关系良好(r=0.9999),平均加样回收率为98.62%,RSD=4.69%。结论:该方法稳定、结果可靠、重复性好,可作为保济丸质量控制标准之一。     

姜三七挥发油指纹图谱研究

目的建立姜三七挥发油气相色谱指纹图谱。方法采用水蒸汽蒸馏法提取挥发油,色谱柱为DB-1701（30m×0.25μm×0.32 mm）毛细管柱,检测器为FID检测器,采用程序升温,柱温110℃,保持5 min,以4℃min-1的升温速率升至160℃,保持3 min;再以2℃min-1的升温速率升至180℃,保持3 min;最后以3℃min-1的升温速率升至240℃,保持3 min。结果依据11批药材的指纹图谱数据建立共有模式,得到共有峰10个。结论本测定方法为姜三七药材的质量评价提供了科学依据。     

气相色谱法测定血栓心脉宁胶囊中麝香酮含量

目的：建立血栓心脉宁胶囊中麝香酮的含量测定方法。方法：采用DB-FFAP色谱柱（30 m×0.25 mm×0.2 μm）;起始温度为130 ℃,保持5 min,以2 ℃?min-1的速率升温至180 ℃,保持8 min,再以20 ℃?min-1的速率升温至250℃,保持5 min;氢火焰离子化检测器（FID）,温度250 ℃。结果：麝香酮进样量在0.01 μg～0.10 μg范围内线性关系良好（r = 0.999 7）,平均回收率99.31 %（RSD=0.7 %）。结论：本方法简便、准确,重现性好,可以用于血栓心脉宁胶囊的质量控制。     

GC-MS/MS测定头孢拉定原料中N,N-二甲基甲酰胺及N-甲基乙酰胺的残留量

摘要：目的:建立GC-MS/MS测定头孢拉定原料中N,N-二甲基甲酰胺（DMF）及N-甲基乙酰胺（NMAC）的残留量的方法。方法:色谱条件Agilent VF-WAXms毛细管柱（30 m×0.25 mm, 0.25μm）,进样口温度为250℃;载气为高纯氦气,进样口为恒流模式,流速1.0 ml·min-1;分流进样,分流比10∶1。程序升温:初始温度50℃,保持1min,以10℃·min-1的速率升至180℃,保持2 min,再以20℃·min-1的速率升至240℃,保持10 min。质谱条件离子源为电子轰击源（EI）,离子源温度280℃。碰撞气为氮气,流速1.5 ml·min-1。质谱传输接口温度250℃。质谱监测模式为多反应监测（MRM）。结果:DMF在0.109～7.270μg·ml-1内与其峰面积呈良好的线性关系（r=0.999 9）,加标回收率为92.70%（RSD=4.28%,n=6）;NMAC在0.109～7.280μg·ml-1内与其峰面积呈良好的线性关系（r=0.999 9）,加标回收率为109.89%（RSD=4.24%,n=6）。结论:本方法经方法学验证,可用于测定头孢拉定中DMF及NMAC的残留量。     

Nachweis einiger Heilmittel in der Kniegelenksynovialflüssigkeit

Zusammenfassung Mittels Gaschromatographie und Dünschichtchromatographie wiesen die Autoren 11 Substanzen nach, welche durch Injektion oder nach Verabreichung per os in die Kniegelenksynovialflüssigkeit eindrangen. In ihrer Aufstellung konnten sie eine direkte Beziehung zwischen Struktur sowie chemischphysikalischen Eigenschaften der Substanz und ihrer Fähigkeit, aus dem Blut in die Kniegelenksynovialflüssigkeit einzudringen, nicht nachweisen, außer der Tatsache, daß Substanzen mit starker Affinität zu Eiweißstoffen erst in höheren Dosen nachweisbar waren.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

Emerging drugs for epilepsy

Epilepsy affects ≤ 1% of the world's population. Antiepileptic drugs (AEDs) are the mainstay of treatment, although more than a third of patients are not rendered seizure free with existing medications. Uncontrolled epilepsy is associated with increased mortality and physical injuries, and a range of psychosocial morbidities, posing a substantial economic burden on individuals and society. Limitations of the present AEDs include suboptimal efficacy and their association with a host of adverse reactions. Continued efforts are being made in drug development to overcome these shortcomings employing a range of strategies, including modification of the structure of existing drugs, targeting novel molecular substrates and non-mechanism-based drug screening of compounds in traditional and newer animal models. This article reviews the need for new treatments and discusses some of the emerging compounds that have entered clinical development. The ultimate goal is to develop novel agents that can prevent the occurrence of seizures and the progression of epilepsy in at risk individuals.     

盐酸达泊西汀中甲磺酸甲酯、甲磺酸乙酯及甲磺酸异丙酯的顶空毛细管GC-ECD法测定

建立了衍生化顶空毛细管气相色谱-电子捕获检测器(ECD)法测定盐酸达泊西汀中的甲磺酸甲酯(MMS)、甲磺酸乙酯(EMS)和甲磺酸异丙酯(IMS).应用碘化钠衍生技术,使用PW-5毛细管柱,载气为氮气,ECD检测,程序升温.MMS、EMS和IMS分别在0.03～0.30、0.05～0.50和0.05～0.50 μg/ml浓度范围内线性关系良好,平均回收率分别为63.5％、100.3％和96.2％,最低检测限分别为0.30、0.50和0.50 ng/ml.     

Lung disease and PKCs

The lung offers a rich opportunity for development of therapeutic strategies focused on isozymes of protein kinase C (PKCs). PKCs are important in many cellular responses in the lung, and existing therapies for pulmonary disorders are inadequate. The lung poses unique challenges as it interfaces with air and blood, contains a pulmonary and systemic circulation, and consists of many cell types. Key structures are bronchial and pulmonary vessels, branching airways, and distal air sacs defined by alveolar walls containing capillaries and interstitial space. The cellular composition of each vessel, airway, and alveolar wall is heterogeneous. Injurious environmental stimuli signal through PKCs and cause a variety of disorders. Edema formation and pulmonary hypertension (PHTN) result from derangements in endothelial, smooth muscle (SM), and/or adventitial fibroblast cell phenotype. Asthma, chronic obstructive pulmonary disease (COPD), and lung cancer are characterized by distinctive pathological changes in airway epithelial, SM, and mucous-generating cells. Acute and chronic pneumonitis and fibrosis occur in the alveolar space and interstitium with type 2 pneumocytes and interstitial fibroblasts/myofibroblasts playing a prominent role. At each site, inflammatory, immune, and vascular progenitor cells contribute to the injury and repair process. Many strategies have been used to investigate PKCs in lung injury. Isolated organ preparations and whole animal studies are powerful approaches especially when genetically engineered mice are used. More analysis of PKC isozymes in normal and diseased human lung tissue and cells is needed to complement this work. Since opposing or counter-regulatory effects of selected PKCs in the same cell or tissue have been found, it may be desirable to target more than one PKC isozyme and potentially in different directions. Because multiple signaling pathways contribute to the key cellular responses important in lung biology, therapeutic strategies targeting PKCs may be more effective if combined with inhibitors of other pathways for additive or synergistic effect. Mechanisms that regulate PKC activity, including phosphorylation and interaction with isozyme-specific binding proteins, are also potential therapeutic targets. Key isotypes of PKC involved in lung pathophysiology are summarized and current and evolving therapeutic approaches to target them are identified.