HPLC法测定茵栀黄软胶囊中黄芩苷、栀子苷和绿原酸的含量

目的测定茵栀黄软胶囊中的 3种有效成分 ,黄芩苷、栀子苷、绿原酸的含量。方法HPLC法 ,Irregular HC18(2 5 0 . 0mm× 4 6mm ,10 μm)色谱柱。黄芩苷流动相 :甲醇 水 磷酸 (V∶V∶V =4 7. 0∶5 .3 0∶0. 2 ) ,流速 :1 0mL·min-1,检测波长 :2 80nm ;栀子苷流动相 :乙睛 水 (V∶V =15∶85 ) ,流速 :1 0mL·min-1,检测波长 :2 38nm ;绿原酸流动相 :乙睛 磷酸溶液 (w =0 . 4 % )(V∶V =13∶87) ,流速 :1 0mL·min-1,检测波长 :32 7nm。结果黄芩苷在 2 7 5～ 137 5mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =6 4. 83× 10 4ρ - 1 6. 96× 10 .5 ,r =0 . 9998,平均回收率为 99 4 6 % (RSD =1 0 1% ) ;栀子苷在 16 .5～ 82 . 5mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =8 794× 10 .5ρ - 4 . 116× 10 2 ,r =0 . 9999,平均回收率为 10 0 . 37% (RSD =1 4 .0 % ) ;绿原酸在 2 4～ 12 0mg·L-1内质量浓度与峰面积具有良好的线性关系 ,线性回归方程为A =2 4 88× 10 4ρ - 9 2 4 4× 10 4,r =0 9999,平均回收率为 99 38%(RSD =1. 89% )。结论测定方法可用于茵栀黄软胶囊的质量控制。     

高效液相色谱法测定复方荔枝草颗粒剂中高车前苷含量

目的 :建立测定复方荔枝草颗粒剂中高车前苷含量的高效液相色谱法。方法 :以KF -C18(2 5 0mm× 4 6mm ,10 μm)为分析柱 ,流动相为甲醇 -水 -pH 3 5的 1 0mol·L-1磷酸盐缓冲液 (4 0∶5 5∶5 ) ;柱温为 45℃ ;检测波长为 335nm ;流速为 1 0mL·min-1,采用面积外标法。结果 :线性范围 3 12× 10 -3 ～ 0 2 0 μg ,平均回收率为 96 96 %～ 10 1 5 % ,RSD <0 6 9% (n =3)。结论 :本法简便、灵敏、重现性好 ,可用于测定该颗粒剂高车前苷的含量和质量标准的控制。     

高效液相色谱法测定奥卡西平及片剂的含量和有关物质

目的 :用高效液相色谱法测定奥卡西平及片剂的含量和有关物质。方法 :采用DiamonsilC18(2 0 0mm× 4.6mm ,5 μm)色谱柱 ,流动相 :乙腈 0 .0 5mol·L 1磷酸二氢钾 (磷酸调 pH为 3.0 ) (4 0 :6 0 ) ,检测波长 :2 5 6nm ,柱温 :40℃ ,流速 :1.0ml.min 1,峰面积外标法。结果 :在 12 .5～ 112 .5 μg .ml 1的奥卡西平浓度范围内 ,峰面积与浓度呈良好的线性关系 ,回归方程 :Y =3.2×10 5C - 2 .6 1× 10 3 相关系数r=0 .9996 ;片剂中奥卡西平平均回收率为 99.7% (n =5 ) ,RSD =0 .33%。结论 :方法简便 ,快速 ,准确。可同时分离和测定奥卡西平原料及其片剂中各杂质及主药含量     

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盐酸左旋咪唑片的含量

目的　以西咪替丁为内标 ,建立RP -HPLC法测定盐酸左旋咪唑片的含量。方法　选用ODS -C18柱 (5 μm ,4 6mm× 15 0mm) ;流动相 :甲醇 水 二乙胺 磷酸 (36∶6 4∶0 1∶0 0 6 ) ,pH7 0 ;检测波长 :2 15nm ;流量∶1 0ml·min-1;进样体积∶2 0 μl。结果　进样量在 0 32～ 1 6 μg范围内 ,相关性良好 ,回归方程 :Y =2 2 0 1X +7 4× 10 -3 ,r=0 9998。平均回收率为 99 8% (n =5 )。结论　本法简便、快速、准确。     

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。     

高效液相色谱法测定呱仑酸钠的含量及有关物质

目的 :建立一种用高效液相色谱法测定呱仑酸钠的含量及有关物质的方法。方法 :在InertsilCN - 3柱上 ,以磷酸盐缓冲液 (pH =7) -乙腈 (5 0∶5 0 )为流动相 ,于 2 90nm波长处检测 ,流速为 1 0mL·min-1。结果 :呱仑酸钠的浓度在1 0～ 6 0 μg·mL-1范围内线性关系良好 ,回归方程 :A =6 2 0 0× 10 5C 6 374× 10 4 ,r =0 9996。精密度试验RSD =0 2 9% (n =6 ) ,最低检出限为 0 2 4ng。有关物质可检出 2个杂质。结论 :本方法简单、快速、结果准确     

HPLC测定复方阿苯达唑片的含量

目的　用HPLC法测定复方阿苯达唑片中阿苯达唑和双羟萘酸噻嘧啶的含量。方法　采用硅胶柱 ,以乙腈 -混合液[水 -乙酸 -二乙胺 (2 .5∶2 .5∶1) ](5 4∶1)为流动相 ,检测波长 2 88nm。结果　阿苯达唑的线性范围为 0 2～ 0 6 μg ,回归方程为 :Y =1.832× 10 6X +7.2 84× 10 3 (r=0 .9998) ;双羟萘酸噻嘧啶的线性范围为 0 .8～ 2 .4 μg ,回归方程为 :Y =1 2 5 5× 10 6X -1 736× 10 4(r=0 .9995 )。结论　所用方法简便、快速 ,准确、可靠。     

高效液相色谱法测定盐酸左氧氟沙星的含量

目的 　建立 HPL C法测定盐酸左氧氟沙星含量的方法。 方法 　色谱柱 :Hypersil ODS2 ( 5 μm,15 0 mm× 4.6mm) ,流动相 :水 -甲醇 ( 3∶ 1)含 3 .4%磷酸氢二钾 ( w/v) ,0 .8%磷酸 ( v/v) ,0 .7%已烷磺酸钠 ( w/v)。流速 1.0 m l· min- 1 ,检测波长 2 93 nm,柱温为 40℃ ,进样量 10μL。结果　在 5 .89× 10 - 2 mg· m L- 1 -13 .74× 10 - 2 mg·m L- 1浓度范围内线性良好。回归方程 Y=5 .5 60× 10 4 X-118.18,r=0 .9998,平均回收率为99.8% ,RSD=0 .5 %。 结论 　本法简便准确 ,重现性好。     

HPLC测定盐酸小檗碱片的含量

目的　建立盐酸小檗碱片的含量测定方法。方法　采用HPLC法 ,选用InertsilODS - 3C18色谱柱 (2 5 0mm× 4 .6mm ,5μm) ,0 .0 33mol·L-1KH2 PO4溶液 -乙腈 (6 5∶35 )为流动相 ,检测波长为 2 6 5nm。结果　盐酸小檗碱在 0 .2～ 1.6 μg·ml-1浓度范围内线性关系良好。回归方程为 :A =4 .2 12× 10 6C - 1.0 0 9× 10 5(r=0 .9999)。结论　所用方法简便、快速 ,结果准确。     

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.