HPLC法测定精制冠心口服液中丹参素的含量

建立了反相HPLC测定精制冠心口服液中的丹参素的含量测定方法。采用C18柱 ,水 -甲醇 -二甲基甲酰胺 -冰醋酸 ( 90∶4∶4∶2 )为流动相 ,检测波长 2 81nm ,线性范围为 0 .0 2 72～ 0 .2 2 4 8mg/ml(r=0 .9999,n =5) ,回收率为 98.4 % ,RSD =0 .8%     

RP-HPLC法测定抗病毒口服液中连翘苷含量

采用 RP- HPL C法测定抗病毒口服液中连翘苷含量。固定相为 Nova- Pak C18反相柱 ;流动相为甲醇 -水 -磷酸 (4 3∶ 57∶ 0 .2 ) ;检测波长为 2 77nm。该方法的线性范围为 0 .4 2～ 4 .2 3μg(r =0 .9999) ,平均回收率为95.6 % ,RSD =3.0 1% (n =6 )。     

RP-HPLC测定上感口服液中丹皮酚含量

应用RP -HPLC测定上感口服液中丹皮酚的含量。采用ODS色普柱 ( 2 5 0mm× 4 6mm ,5 μm) ,甲醇-水 -冰醋酸 ( 65∶35∶0 5 )为流动相 ,检测波长为 2 74nm。丹皮酚在 2 5～ 30 μg ml-1浓度范围内呈良好线性关系 (r =0 9999) ,平均回收率为 95 7%,RSD =2 1%(n =6)。方法准确、灵敏 ,回收率高。     

薄层扫描法测定降脂通脉口服液中阿魏酸的含量

目的　测定降脂通脉口服液中阿魏酸的含量。方法　采用薄层扫描法测定降脂通脉口服液中阿魏酸的含量。以苯 -冰醋酸 -氯仿 (6∶ 0 .5∶ 5 )为展开剂 ,单波长反射法锯齿扫描 ,扫描波长为 3 2 5 nm。结果　样品平均回收率为 1 0 0 % ,精密度 RSD =0 .6 7% (n =6 )。结论　方法灵敏 ,稳定性好 ,可作为该制剂质量控制指标     

RP-HPLC测定盐酸西替利嗪的含量及相关物质

目的　采用RP -HPLC法测定盐酸西替利嗪的含量及其有关物质。方法　采用ODS色谱柱 (5 μm ,4 .6mm× 15 0mm) ,流动相为乙腈 -水 -冰醋酸 (36∶6 4∶0 .1) ,流速 1.0ml·min-1,检测波长 2 2 9nm ,柱温为室温 (2 5℃ )。结果　盐酸西替利嗪测定的线性范围为 12 .5～ 15 0 μg·ml-1(r=0 .9998,n =6 ) ;日内RSD =0 .36 % (n =5 ) ,日间RSD =0 .6 4 % (n =5 ) ;最低检出限 0 .3ng。结论　所用方法简便、准确 ,专属性好     

HPLC测定川产六种鹿蹄草中高熊果苷的含量

目的　对川产 6种鹿蹄草中的高熊果苷进行含量测定。方法　用HPLC ,色谱柱SynchromSi(5 μm ,15 0mm× 4 .6mm) ,流动相为正己烷 -醋酸乙酯 -甲醇 (30∶10∶9) ,检测波长 2 80nm。结果和结论　线性范围为 0 .5 2 4～2 .6 4 μg(r=0 .9997) ,平均回收率 96 .6 8% ,RSD =3.72 %。该方法可行     

高效液相法测可乐定贴片的释放度

目的　建立一种采用高效液相色谱检测可乐定贴片的释放度的方法。方法　采用 KP1 0 0 - SC1 8色谱柱 (2 5 mm× 4 .6 mm ) ,流动相为乙腈∶水∶三乙胺 =5 0∶ 5 0∶ 0 .0 5 (用稀磷酸调节至 p H4 .8) ,UV检测波长为 2 0 0nm。结果　该法平均回收率为 1 0 0 .4 3% ,RSD为 1 .4 3% (n=5 )。结论　该法操作简便、快速     

HPLC测定克拉霉素及其制剂的含量

目的　采用HPLC法测定克拉霉素及其制剂的含量。方法　C1 8或C8色谱柱 (4 .6mm× 2 5 0mm ,5 μm) ,流动相分别为磷酸二氢钾溶液 (0 .0 6 7mol·L- 1 ) -甲醇 (4 0 0∶6 0 0 ) (pH 4 .0 )和磷酸二氢钾溶液 (0 .0 6 7mol·L- 1 ) -乙腈 (5 5∶4 5 ) ,检测波长 2 10nm ,均采用外标法。结果　 3种方法线性范围均为 0 .0 2 5～ 2 .0mg·ml- 1 (r=0 .9999) ,平均回收率为 10 0 .2 % ,RSD =0 .4 8% (n =6 )。结论　 3种方法的分离效果均较好 ,没有明显差异 ,其中方法b较为适宜。     

高效液相色谱法测定益宫散结口服液中芍药苷的含量

目的 :应用高效液相色谱法对益宫散结口服液进行含量测定。方法 :选用HypersilODS 2分析柱 (2 5 0mm×4 .6mm ,5 μm) ,乙腈 - 0 .0 5mol·L-1磷酸二氢钾 (13∶87)为流动相 ,检测波长为 2 30nm ,流速 1.0ml·min-1。结果 :线性范围为1.12～ 13.4 4 μg(r=0 .9997) ,平均回收率为 97.7% ,RSD为 1.1%。结论 :本法简便、灵敏、准确。     

高效液相色谱法测定牛葛口服液中葛根素的含量

目的 　建立牛葛口服液中葛根素的含量测定方法。方法 　用 Nova-Pak C1 8色谱柱 ( 3 .9mm× 15 0 mm,4μm)为固定相 ,甲醇 -水 2 5∶ 75 ( V/V)为流动相 ,检测波长为 2 5 0 nm。 结果 　葛根素 0 .40 4～ 2 .0 2 0μg范围内呈良好的线性关系 ,r=0 .9999;葛根素的加样回收率为 99.2 3 %,RSD= 1.2 9%;连续进样的精密度是 RSD=0 .2 6%。 结论 　该方法能消除其它成分的干扰 ,准确可靠、重现性好 ,操作简便快速     

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.