HPLC法测定华山参滴丸中东莨菪碱、阿托品及东莨菪内酯的含量

目的:建立HPLC法测定华山参滴丸中东莨菪碱、阿托品及东莨菪内酯的含量。方法:采用资生堂CAPCELL-PAK C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-甲醇-磷酸氢二钠缓冲液(15∶4∶81)为流动相,流速1.0 mL·min-1,东莨菪碱、阿托品检测波长210 nm(0～15 min),东莨菪内酯检测波长为344 nm(15.1～30 min),柱温30℃。结果:东莨菪碱、阿托品及东莨菪内酯的线性范围分别为0.04～3.95,0.04～4.10,0.05～0.54μg(r=0.9999);平均回收率(n=6)分别为97.58%(RSD=1.3%),98.65%(RSD=1.3%),98.42%(RSD=1.8%)。结论:本文方法简便、准确,可以用于华山参滴丸中东莨菪碱、阿托品及东莨菪内酯的含量测定。     

华山参中东莨菪内酯的含量测定方法研究

目的:建立高效液相色谱法测定华山参中东莨菪内酯含量的方法。方法:色谱柱:Agilent ODS C18柱(250 mm×4.6 mm,5μm),流动相:甲醇-0.3%磷酸溶液(30∶70),柱温:35℃,流速:1.0 mL.min-1,测定波长:344 nm。结果:东莨菪内酯的线性范围:9.84~1476.0 ng(r=0.99998);平均回收率在97.2%~100.7%,RSD为1.4%(n=6)。结论:本方法准确、可靠,重复性好,可用于华山参药材的质量控制。     

HPLC同时测定桑白皮中绿原酸、东莨菪内酯、白藜芦醇、桑色素4种成分的含量

目的:分析HPLC同时测定桑白皮中绿原酸、东莨菪内酯、白藜芦醇、桑色素4种成分含量的有效性.方法:对桑白皮中桑色素、白藜芦醇、东莨菪内酯、绿原酸四种成分含量采用HPLC法进行测定,并对其测定结果进行分析.结果:平均加样回收率在98.4％～99.4％之间,12h内,供试品具有良好稳定性,白藜芦醇在产地为湖北桑白皮中的含量最多,桑色素、绿原酸、东莨菪内酯在产地为河南桑白皮中的含量最多.结论:HPLC同时测定桑白皮4种成分含量的准确度、精密度高.     

桑白皮流浸膏的质量标准

目的：建立桑白皮流浸膏质量标准。方法：用薄层色谱法进行鉴别;用HPLC法对东莨菪内酯进行含量测定。结果：鉴别斑点清晰;东莨菪内酯平均加样回收率为102．6％,RSD为1．03％（n=6）。结论：方法简便、准确,专属性强,可用于桑白皮流浸膏的质量控制。     

HPLC法测定丁公藤中东莨菪素及东莨菪苷的含量

目的测定丁公藤中抗风湿成分东莨菪素及东莨菪苷的含量.方法采用HPLC法,Spherisorb 50DS(2)色谱柱,流动相甲醇-水(1100),检测波长347nm.结果可同时测定2成分含量;东莨菪素在0.288-1.440μg、东莨菪苷在0.384～1.920μg范围内呈现良好线性关系,平均回收率分别为101.5%;98.7%;RSD分别为1.92%;1.58%(n=5).结论方法简便、可靠,可同时测定该生药中2个抗风湿成分的含量.     

退黄藤中东莨菪内酯的分离纯化及含量测定

目的 分离纯化退黄藤中的东莨菪内酯并测定其含量.方法 采用硅胶柱色谱分离纯化退黄藤中的东莨菪内酯,并根据理化性质及光谱数据鉴定其结构;采用HPLC法测定其含量,色谱柱为Zorbax Eclipse XDB-C1s柱(250 mm ×4.6 mm,5μm),流动相为甲醇-0.1％冰乙酸(39∶61),流速1.0 mL·min-1,检测波长345 nm.结果 东莨菪内酯3.11 ～31.1 μg·mL-1与峰面积呈良好的线性关系(r =0.9999),平均回收率为99.29％,RSD=1.40％(n=6).结论 所用方法简便、准确、快速,可用于退黄藤药材的质量控制.     

双波长薄层扫描法测定地骨皮中莨菪亭含量

本文用双波长薄层扫描法首次测定了５种商品地骨皮药材中莨菪亭的含量，以山西２产地骨皮的含量最高。     

双波长扫描法测定复方羊角胶囊中东莨菪内酯的含量

采用高效硅胶 G薄层色谱板 ,以氯仿 -丙酮 -甲苯 -冰醋酸 ( 9∶ 0 .5∶ 0 .5∶ 1d)为展开剂 ,双波长反射法锯齿扫描测定 λS=34 5nm,λR=2 65nm,平均回收率为 99.98% ,RSD =0 .4 5% ( n=5) ,胶囊中东莨菪内酯含量为 0 .144‰。     

胃肠宁胶囊定性定量方法研究

目的建立胃肠宁胶囊的质量控制方法。方法采用TLC法定性鉴别,HPLC法测定有效成分东莨菪内酯的含量。结果薄层色谱鉴别中,供试品色谱中,在与对照品、对照药材色谱相应的位置上,显相同颜色的斑点。东莨菪内酯在21.40~214.0μg·m L-1内与峰面积呈良好的线性关系(r=0.999 5),平均回收率为100.4%,RSD为1.7%。结论所建方法准确可靠、灵敏度高、专属性强,可有效控制胃肠宁胶囊的质量。     

HPLC-荧光检测法测定枸杞子和五子衍宗丸中东莨菪内酯的含量

目的采用高效液相色谱-荧光检测法(HPLC-FLD)测定枸杞子和五子衍宗丸中东莨菪内酯的含量。方法色谱条件:色谱柱为Agilent Extend-C18柱(4.6 mm×250 mm,5μm);流动相为乙腈-0.1%磷酸(18∶82);流速为1.0 m L·min?1;柱温30℃;荧光检测器激发波长343 nm,发射波长458 nm。结果东莨菪内酯在41.63~2 082 pg内线性关系良好(r=1),回归方程Y=44 095X–44 660,在枸杞子药材中平均回收率为101.1%,RSD为2.2%(n=9),在五子衍宗丸中平均回收率为102.6%,RSD为1.1%(n=9)。宁夏产的枸杞子东莨菪内酯含量高于其他产地。结论该方法快速、简便、灵敏,专属性、重复性良好,有助于评价枸杞子的道地性以及初步区分样品的来源,适用于枸杞子药材和五子衍宗丸中君药枸杞子的质量控制与评价。     

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.