HPLC法测定醋氯芬酸片有关物质影响因素

目的　HPLC法测定醋氯芬酸片有关物质影响因素。方法　以WatersODSC18为色谱柱 ,醋酸钠缓冲液 乙腈 (40∶6 0 )为流动相 ,检测波长 2 75nm。结果　在 pH2 5的溶液中处理样品 ,样品随放置时间延长 ,发生水解 ,影响检测结果。结论　样品在酸性条件下易发生水解 ,在进行含量测定或有关物质检查时 ,应及时测定。     

高效液相色谱法测定复方辛伐他汀烟酸缓释片的有关物质

目的 建立复方辛伐他汀烟酸缓释片有关物质检查的HPLC方法.方法 采用C18柱,以乙腈-0.1%磷酸溶液(50∶50)为流动相A,0.1%磷酸的乙腈溶液为流动相B,梯度洗脱,对辛伐他汀的有关物质进行检测;以乙腈-0.05mol·L-1磷酸二氢钠溶液(磷酸调pH至2.5)(1∶99)为流动相,对烟酸进行检测.结果 在建立的色谱条件下,辛伐他汀、烟酸峰与其相关杂质峰均能完全分离.结论 本法简便、准确、专属性强,可用于本品的有关物质检查.     

高效液相色谱法测定蛋氨酸的有关物质

目的:建立高效液相色谱法测定蛋氨酸的有关物质.方法:采用C18柱,以醋酸盐缓冲液(pH6.40)-60%乙腈(87:13)为流动相,检测波长:254 nm,流速:1.0 mL·min-1,柱温:38℃.结果:蛋氨酸峰与有关物质峰能很好地分离,分离度符合要求.结论:本法简便、灵敏度高,可用于蛋氨酸有关物质的测定.     

HPLC法测定克拉维酸钾有关物质

建立HPLC法,以进一步用液相色谱-质谱联用技术检查并推证克拉维酸钾中的有关物质。采用HPLC法测定,液相色谱条件为:采用ZORBAX ODS色谱柱,流动相A为0.01mol.L-1乙酸铵,流动相B为流动相A-乙腈(1∶1),流速:1mL.min-1,检测波长:230nm。克拉维酸钾浓度在5~160μg.mL-1范围内与峰面积呈良好线性关系(r=0.9999),最低检测限为0.3μg.mL-1。本法简便、准确、灵敏度高,适用于克拉维酸钾中有关物质的测定。     

HPLC梯度洗脱法检查甲睾酮喷雾剂中的有关物质

目的 建立检查甲睾酮喷雾剂中有关物质的方法.方法 采用HPLC梯度洗脱法,色谱柱为VP-C18柱(250 mm×4.6 m,5 μm);以甲醇-乙腈-水(33:22:45)为流动相A,乙腈为流动相B,梯度洗脱;检测波长241 nm;柱温35℃;流速1.0 ml·min-1.结果 在选定的色谱条件下,主成分与有关物质能完全分离,各杂质峰分离良好,最低检测限为0.06 ng.结论 所建方法专属性强、灵敏度高、重复性好,可用于检查甲睾酮喷雾剂的有关物质.     

HPLC法检测齐多夫定的有关物质

目的:建立了齐多夫定的有关物质[有关物质B(3’-氯-3’-脱氧胸苷)、有关物质C(胸苷)]的HPLC检测方法。方法:采用Lichrospher-C18色谱柱(250 mm×4．6 mm,5μm);流动相A为水,流动相B为甲醇,采用梯度洗脱,10 min后流动相 A在40 min内从70％降至30％,流速1．0 mL·min-1,检测波长265 nm。结果:有关物质B、C和齐多夫定的最低检测限量分别为4．4,2．6,4．0 ng,齐多夫定与各杂质分离良好。结论:本法简便快速,灵敏度高,准确可靠。     

高效液相色谱法测定注射用HB的有关物质

目的 采用高效液相色谱法检查HB的有关物质.方法 色谱柱用C18s柱(250 mm×4.6 mm,5μm),柱温为40℃,检测波长为210 nm,流动相为0.01 mol/L磷酸二氢钠-甲醇-异丙醇(97:2:1),流速1 mL/min.结果 样品中有关物质小于0.5%.结论 HPLC法检查注射用HB中有关物质简便、准确.     

HPLC测定头孢西丁钠有关物质

目的 建立头孢西丁钠有关物质的高效液相测定方法.方法 采用CLC-Pheny1色谱柱(5 μm,150 mm×6.0 mm),以水-乙腈(80:20)为流动相;流速1.0 ml/min,检测波长为235 nm.结论 本方法准确性好、专属性强,适用于头孢西丁钠有关物质的测定.     

盐酸非索非那定有关物质测定方法的建立

目的　建立盐酸非索非那定有关物质的HPLC分析方法。方法　采用苯基柱(250mm×4. 6mm, 5μ),流动相: 0. 5%磷酸二氢钠水溶液(pH4. 0) 乙腈三乙胺(60∶40∶0. 3);流速1. 5ml/min;检测波长220nm。采用归一化法测定盐酸非索非那定有关物质的含量。结论　本方法简便、快速、灵敏,可用于盐酸非索非那定有关物质的测定。     

高效液相色谱法测定右旋布洛芬凝胶中的有关物质

目的:建立高效液相法测定右旋布洛芬凝胶中有关物质的方法。方法:测定左旋布洛芬的色谱条件CHI-TBB(4.6mm×250mm,5μm)手性柱,流动相为正己烷-叔丁甲醚-冰醋酸(87∶13∶0.1),检测波长为263nm,流速为1.0mL.min-1,柱温为40℃;测定其他有关物质的色谱条件为Hypersil ODS2色谱柱,流动相为乙腈-水(用磷酸调节pH至3.0)(58∶42),流速为1.0mL.min-1;检测波长为263nm;柱温为35℃。结果:有关物质与右旋布洛芬主峰有良好的分离,3批样品的检测符合右旋布洛芬凝胶中有关物质检查的要求。结论:2种方法可用于右旋布洛芬凝胶中有关物质的检测。     

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.

---

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.