高效液相色谱-蒸发光散射检测法测定莕菜中白桦脂酸的含量

目的:建立高效液相色谱-蒸发光散射检测法(HPLC-ELSD法)测定莕菜中白桦脂酸的含量。方法:采用Hypersil C18(4.6 mm×250 mm,5μm)色谱柱,流动相为甲醇-0.2%甲酸(V∶V=80∶20),体积流量为1.0 ml/min;柱温为30℃;蒸发光散射检测器参数:漂移管温度为40℃,氮气流速为2.0 L/min。结果:白桦脂酸在0.130~0.650μg,线性关系良好,平均回收率为99.17%。结论:HPLC-ELSD法简便、准确、重现性好,可用于莕菜的质量控制。     

HPLC-蒸发光散射检测法测定不同产地酸枣仁中白桦脂酸的含量

目的建立以高效液相色谱-蒸发光散射检测法测定酸枣仁中白桦脂酸含量的方法。方法色谱柱为Agilent C18(250mm×4.6mm,5μm),流动相为甲醇-水-三乙胺(用冰醋酸调至pH=5.7,86∶14∶0.03),流速为1.0mL.min-1,柱温为25℃,进样量为20μL,漂移管温度为80℃,气体(氮气)流速为2.0L.min-1。结果白桦脂酸检测浓度在10.10~161.60μg·mL-1范围内线性关系良好(r=0.9995,n=6);平均加样回收率为97.95%(RSD=0.25%)。结论本方法简便、准确、重现性好。     

HPLC-ELSD法测定龙牡壮骨颗粒中黄芪甲苷的含量

目的:研究龙牡壮骨颗粒中黄芪甲苷的含量测定方法.方法:高效液相色谱-蒸发光散射检测法.色谱柱为Diamonsil C18,4.6mm×250mm,5μm;流动相为甲醇-水(75:25);流速为1.0mL·min-1;柱温为30℃;检测器为Varian 380 - LC型蒸发光散射检测器.结果:该方法能很好分离被测组分与...     

HPLC-ELSD法测定复方石韦胶囊中黄芪甲苷的含量

目的采用高效液相色谱-蒸发光散射检测器(HPLC-ELSD)法测定复方石韦胶囊中黄芪甲苷的含量。方法采用Hypersil ODS2(4.6 mm×150 mm,5μm)色谱柱;流动相:乙腈-水(30∶70);流速:1.0 mL.min-1;柱温:25℃;蒸发光散射检测器条件,漂移管温度:50℃。结果黄芪甲苷在1.334～9.336μg(r=0.999 9)的范围内,呈良好的线性关系。平均加样回收率为100.4%(n=9),RSD为1.61%。结论本方法操作简便、准确、稳定、灵敏度高,可作为该制剂的质量控制方法。     

亲水作用色谱-蒸发光散射法测定益母草中盐酸水苏碱的含量

目的:建立亲水作用色谱-蒸发光散射检测器联用测定益母草中盐酸水苏碱含量的方法。方法:采用HILIC柱(250mm×4.6 mm,5μm);乙腈-0.2%冰醋酸溶液(80∶20)为流动相;Alltech2000蒸发光散射检测器:漂移管温度80℃,气体流速2.0 L.min-1;流速0.5 mL.min-1。结果:盐酸水苏碱进样量在0.536～10.713μg范围内呈良好的线性关系,平均回收率为101.9%,RSD为1.4%。结论:此方法简便、灵敏度高,重现性好,可用于益母草的含量测定。     

HPLC-ELSD测定威灵仙中齐墩果酸的含量

目的 建立威灵仙中齐墩果酸的高效液相色谱-蒸发光散射法测定方法。方法 采用 SumFire TM C18(4.6 mm×250 mm,5 μm)色谱柱,柱温40 ℃;乙腈-水(85∶15)为流动相,流速1.0 mL·min-1;蒸发光散射检测器漂移管温度85 ℃,空气流速2.3 L·min-1。结果 齐墩果酸在0.214～1.92 μg内线性关系良好,r =0.999 9,平均回收率为98.8%,RSD为0.9%(n=6)。结论 该方法简便,快速,准确,可作为威灵仙的质量控制。     

高效液相色谱-蒸发光散射法测定奈替米星含量

目的 　建立高效液相色谱 -蒸发光散射法测定奈替米星含量。方法 　采用 ZORBAX Extend-C1 8( 4 .6× 2 5 0 mm,5μm)柱 ,以 0 .2 mol· L - 1三氟醋酸 -甲醇 ( 92∶ 8)为流动相 ,流速 0 .6ml· min- 1 ;蒸发光散射检测器 :漂移管温度 110℃ ,载气流速为 2 .8L· min- 1 。 结果 　奈替米星在0 .5～ 5 μg范围内呈良好的线性关系 ,r=0 .9999;平均回收率为 98.7%,RSD=1.8%( n=9)。结论 　本法简便、快速 ,结果准确、可靠 ,重现性好     

高效液相色谱-蒸发光散射检测法同时测定木瓜中齐墩果酸和熊果酸含量

目的:建立高效液相色谱-蒸发光散射检测法同时测定中药木瓜中齐墩果酸和熊果酸含量.方法:固定相为YMC C18(4.6 mm×250 mm,5 μm)色谱柱,柱温:35 ℃;流动相:乙腈-水(88∶12),流速:0.8 mL·min-1;蒸发光散射检测器检测,漂移管温度90 ℃,气体(空气)流速2.30 L·min-1.结果:齐墩果酸在0.20～2.01 μg范围内(r=0.999 6)线性关系良好,熊果酸在0.20～2.05 μg范围内(r=0.999 8)线性关系良好.木瓜中齐墩果酸和熊果酸的回收率分别为99.2%和97.8%,RSD分别为2.2%(n=5)和1.4%(n=5).结论:方法简便、准确,重现性好.     

养血饮口服液的质量标准

目的:建立养血饮口服液的质量控制标准。方法:采用薄层色谱法(TLC)对当归和大枣进行定性鉴别;用高效液相-蒸发光散射法测定黄芪甲苷的含量,选用的色谱柱为Luna C18(250 mm×4.6 mm,5μm),流动相为乙腈-水(38∶62),柱温为40℃,流速为0.8 ml·min-1,蒸发光散射检测器漂移管温度为85℃,气体流速2.0 L·min-1。结果:薄层色谱法检出了当归和大枣的特征斑点,黄芪甲苷的线性范围为0.522~4.176μg(r=0.999 8),平均加样回收率为97.9%,RSD为1.03%(n=6)。结论:该方法易于操作,结果准确,重复性良好,可用于的养血饮口服液质量控制。     

HPLC-ELSD法测定硫酸西索米星氯化钠注射液中西索米星含量

目的　建立高效液相色谱—蒸发光散射检测法测定西索米星的含量。 方法 　采用 ZORBAX Extend— C1 8( 4 .6× 2 5 0 mm,5μm )柱 ,以 0 .2 mol· L - 1三氟醋酸 -甲醇 ( 92∶ 8)为流动相 ,流速为 0 .6ml· min- 1 ;蒸发光散射检测器 :漂移管温度 110℃ ,载气流速为 2 .8L· min- 1。 结果 　西索米星在 1.0 2 1— 10 .2 1μg范围内呈良好线性关系 ,r=0 .9999;平均回收率为 10 1.6% ,RSD=1.1% ( N=9)。 结论 　本法简便快速 ,结果可靠 ,可用于西索米星的含量测定     

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.     

Efficacy of gut lavage,hemodialysis, and hemoperfusion in the therapy of paraquat or diquat intoxication

Clinical and in vitro investigations were carried out to test the efficacy of gut lavage, hemodialysis, and hemoperfusion in the treatment of poisoning with paraquat or diquat. In a patient suffering from diquat intoxication 130 times more diquat was removed by gut lavage 30 h after ingestion than was removed by complete aspiration of the gastric contents.Determination of in vitro clearances for paraquat and diquat by hemodialysis showed that, at serum concentrations of 1–2 ppm, such as are frequently encountered in poisoning in man, toxicologically relevant quantities of herbicide cannot be removed from the body. At a concentration of 20 ppm, on the other hand, hemodialysis proved to be effective, the clearance being 70 ml/min at a blood flow rate of 100 ml/min. The efficacy of hemoperfusion with coated activated charcoal was on the whole better. Especially at concentrations around 1–2 ppm, the clearance values for hemoperfusion were some 5–7 times higher than those for hemodialysis.In a patient suffering from paraquat poisoning, both hemodialysis as well as hemoperfusion were carried out. The in vitro results could be confirmed: At serum concentrations of paraquat less than 1 ppm no clearance could be obtained by hemodialysis while by hemoperfusion with activated charcoal quite high clearance values were measured and the serum level dropped down to zero.

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Zusammenfassung Klinische Untersuchungen und Laboratoriumsversuche wurden durchgeführt, um die Wirksamkeit von Darmspülung, Hämodialyse und Hämoperfusion bei Paraquat- und Deiquat-Vergiftungen zu prüfen.Bei einem Patienten wurde 30 Std nach Deiquat-Aufnahme durch Darmspülung 130mal mehr Deiquat entfernt als durch vollständige Aspiration des Mageninhaltes. In vitro-Versuche ergaben, daß bei Blutserumkonzentrationen von 1–2 ppm, die bei Vergiftungen oft gemessen werden, durch Hämodialyse keine toxikologisch relevanten Paraquat- oder Deiquat-Mengen entfernt werden können. Dagegen erwies sich die Hämodialyse bei 20 ppm und einer Blutumlaufgeschwindigkeit von 100 ml/min mit einer Clearance von 70 ml/min als wirksam. Die Hämoperfusion mit beschicheter Aktivkohle war in diesen Versuchen aber eindeutig überlegen, denn insbesondere bei Konzentrationen um 1–2 ppm waren die Clearance-Werte 5–7mal höher als bei der Hämodialyse.Die in vitro-Ergebnisse wurden bei einem Patienten mit einer Paraquat-Vergiftung bestätigt: Bei Konzentrationen unter 1 ppm war die Hämodialyse wirkungslos, während durch Hämoperfusion relativ hohe Clearance-Werte erreicht wurden, so daß der Serumspiegel rasch unter die Nachweisgrenze abfiel.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine.     

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.     

Steroidal sapogenin contents in some domestic plants

In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.