HPLC法测定苯噻啶的含量

建立苯噻啶对照品含量测定的HPLC方法。色谱柱 :KromasilC18(2 5 0× 4 6mm ,5 μm) ,流动相 :乙腈 -水 -三乙胺 (5 5∶4 5∶0 2 ) ,检测波长 :2 5 6nm ,流速 :1 0ml·min- 1,进样量 :2 0 μl。苯噻啶在浓度为 6 5～ 2 0 8μg·ml- 1浓度范围内线性关系良好。回归方程为A =6 4185 74 +81992 3×C ,r =0 99998。本法简便、灵敏、准确。     

HPLC法测定苯噻啶含量及其有关物质

本文采用HPLC法测定苯噻啶对照品含量及其有关物质。色谱柱KromasilC18(2 5 0× 4 6mm ,5 μm) ,流动相 :乙腈 -水 -三乙胺 (5 5∶4 5∶0 2 ,磷酸调节溶液pH3 5 ) ,检测波长 :2 5 4nm ,流速 :1 0ml·min-1,进样量 :2 0 μl。苯噻啶在浓度 6 5～ 2 0 8μg·ml-1浓度范围内线性关系良好。回归方程A =64185 74 +81992 3C ,r=0 99998。平均回收率 10 0 1% (n =6) ,RSD为 0 5 8%。本法简便、灵敏、准确     

高效液相色谱法测定苯噻啶的含量

目的　建立苯噻啶含量测定的HPLC方法。方法　选用KromasilC18(2 5 0× 4.6mm ,5 μm)色谱柱 ,乙腈 水 三乙胺 (5 5∶45∶0 .2 )为流动相 ,检测波长 :2 5 6nm ,流速为 1.0mL·mL-1,进样量 2 0 μL。 结果　苯噻啶在浓度为 6.5～ 2 0 8μg·mL-1浓度范围内线性关系良好。回归方程为A =64 185 .74+81992 .3×C ,r=0 .99998。结论　本法简便、灵敏、准确。     

HPLC测定磷酸咯萘啶片中主药的含量

目的　建立测定磷酸咯萘啶含量的HPLC方法。方法　选用DiamonsilC1 8(2 50mm× 4 .6mm ,5μm)色谱柱 ,0 .0 8mol·L- 1 磷酸二氢钾 -乙腈 (85∶1 5)为流动相 (含 0 .1 %三乙胺 ,pH3 .0 ) ;检测波长 2 78nm ;流速为 1 .0ml·ml- 1 ;进样量 2 0 μl。 结果　磷酸咯萘啶在浓度 5 .0 8～ 40 6 .4μg·ml- 1 范围内线性关系良好 ;回归方程为A =- 1 2 91 8+1 8657C ,r =0 .9999;平均回收率为 99.8% ,RSD =0 .8% (n =5)。结论　本法简便、灵敏、准确     

复方制剂中双羟萘酸噻嘧啶及阿苯达唑含量测定方法的研究

本文采用双波长法分别测定驱虫药复方制剂的有效成份双羟萘酸噻嘧啶及阿苯达唑，进行了方法学研究、线相关系、加样回收等实验工作，两种效成分的回收率分别为１００．６±０．６８％，９９．２７±０．５９％（ｎ＝２），含量在其标示量的±２０％范围内线性关系良好，分别为ｒ＝０．９９９９，ｒ＝－９９９８。     

HPLC测定土霉素片的含量

目的　测定土霉素片的含量。方法　采用HPLC法 ,C18色谱柱 ,以 0 0 5ml·L-1草酸铵溶液 -二甲基甲酰胺 - 0 2mol·L-1磷酸氢二铵溶液 (75∶2 0∶5 )为流动相 ,检测波长 2 80nm。结果　土霉素在 0 0 1～ 0 15mg·ml-1范围内呈良好的线性关系 ,回归方程为 :Y =2 5 4× 10 7X +2 15× 10 4(r =0 .9996 ,n =7)。平均加样回收率为 98 7% (RSD =1 13% ,n =5 )。结论　方法简便、快速、准确。     

双羟萘酸噻嘧啶咀嚼片抗猪蛔虫的药理效应

目的 :研究双羟萘酸噻嘧啶咀嚼片抗猪蛔虫的药理效应。方法 :将双羟萘酸噻嘧啶咀嚼片、普通片与阿苯哒唑等抗寄生虫药对小猪人工感染蛔虫病理模型进行治疗 ,采用改良加藤氏厚涂片法比较上述各药治疗前后的 EPG(克粪便虫卵数 )和虫卵阴转率。结果 :双羟萘酸噻嘧啶咀嚼片与片剂一样在肠虫营养液中 ,显著引起蛔虫虫体僵硬 ,导致猪蛔虫头颈段活动停止。双羟萘酸噻嘧啶咀嚼片 8m g· kg- 1 和 10 mg· kg- 1 组对小猪感染蛔虫均具有非常显著的驱治效果 ,治疗后虫卵阴转率达 97.2 6 %和 10 0 % (88h)、97.5 1%和 10 0 % (186 h) ,与阴性对照组比较有显著性差异 ;10 m g· kg- 1 组虫卵阴转率及 EPG显著高于阿苯哒唑 (肠虫清 )对照组 ,P<0 .0 5。急性毒性试验结果表明小鼠腹腔注射试验药混悬液 L D50 为 12 7.74～ 16 7.86 m g· kg- 1 ;小鼠累积灌胃给予该药的最小致死量大于 8g· kg- 1。结论 :双羟萘酸噻嘧啶咀嚼片对小猪蛔虫感染具有显著的驱治效应     

HPLC法测定消痛片中延胡索乙素的含量

采用高效液相色谱法测定消痛片的含量。色谱柱为KromasilODSC18(2 5 0mm× 4 6mm ,5 μm) ;流动相为甲醇 -磷酸盐溶液 (6 5∶35 , 磷酸二氢钾 0 1g和磷酸氢二钾 4 8g混合溶解于 5 0 0ml水中 ) ,流速为1ml·min-1,检测波长为 2 82nm。回归方程为Y =7 97× 10 6X - 0 1× 10 5,r =0 9999,平均回收率为97 98% ,RSD为 1 19% (n =5 )。本方法简便、快速 ,重现性好 ,可用于消痛片质量控制。     

HPLC测定克林霉素搽剂的含量

目的　测定克林霉素搽剂的含量。方法　用HPLC法 ,C18色谱柱 ,以磷酸二氢铵溶液 (pH 3.0 ) -甲醇 (2 10∶30 0 )为流动相 ,检测波长 2 14nm。结果　线性范围为 0 .2～ 2 .0mg·ml-1,回归方程为 :Y =9.117× 10 5X +3 10 2× 10 4(r =0 .9999,n =5 )。回收率为 99 7% ,RSD =1 0 2 %。分析方法精密度RSD =1.34% (n =5 )。结论　方法简便、快速、准确。     

HPLC法测定风寒感冒颗粒中的陈皮苷含量

目的 　建立一种风寒感冒颗粒中的陈皮苷含量测定方法。 方法 　样品加入甲醇超声处理 2 0 min,经甲醇稀释后作为供试品溶液。采用HPLC法测定陈皮苷含量。Hypecsil ODS C1 8柱 ( 4 .6mm× 2 5 0 mm,5 μm) ;甲醇 -醋酸 -水 ( 3 5∶ 4∶ 61)为流动相 ;检测波长 λ=2 83 nm。结果 　陈皮苷在 0 .80 14 μg～ 4.0 0 7μg范围内线性关系良好 ,回归方程为 Y=63 2 3 13 X+3 6810 ,r=0 .9996。加样平均回收率为 10 0 .0 2 % ,RSD=2 .70 %。结论 　该方法简单 ,灵敏度高 ,测定结果准确稳定 ,可作为风寒感冒颗粒的质量控制方法。     

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.