HPLC法测定甲磺酸帕珠沙星原料及其制剂含量

目的:采用高效液相色谱法测定甲磺酸帕珠沙星原料及其制剂含量.方法:Hypersil C18(5 μm,4.6 mm×250 mm)色谱柱,0.1%磷酸溶液(加磷酸氢二钾80.5 mg)-乙腈(85:15)为流动相,流速1.0ml·min-1,柱温30℃,检测波长243 nm.结果:甲磺酸帕珠沙星在5～500μg·ml-1内与峰面积呈良好的线性关系.甲磺酸帕珠沙星原料(3批)加样回收率99.2%甲磺酸帕珠沙星注射液加样回收率均值为100.1%;甲磺酸帕珠沙星氯化钠注射液加样回收率均值为99.7%.结论:采用HPLC测定原料及其制剂中甲磺酸帕珠沙星含量方法简便,结果可靠.     

HPLC法测定甲磺酸帕珠沙星注射液中帕珠沙星的含量

目的 建立高效液相色谱法测定帕珠沙星的含量.方法 采用Hypersil ODS2 4.6×200 mm,5μm(依利特)柱,以乙腈-0.67%磷酸二氢钾溶液(用磷酸调节pH值至2.2)-0.05mol·L-1四丁基溴化铵溶液(50 ∶ 432 ∶ 25)为流动相,流速为1.0ml·min-1,紫外检测波长320nm.结果 帕珠沙星在进样量为0.9756～9.756μg范围内呈良好线性关系(r=0.99998,n=6),平均回收率为100.2%,RSD=0.2%(n=9).结论 采用HPLC法测定帕珠沙星的含量,方法简便快速,结果准确,可作为甲磺酸帕珠沙星制剂的质量控制方法.     

高效液相色谱法测定甲磺酸帕珠沙星注射液中右旋体的含量

目的建立甲磺酸帕珠沙星注射液中右旋异构体含量的高效液相色谱测定方法。方法Shim pakCLC ODS柱 (15 0mm× 6 .0mm ,5 μm) ,流动相为L 异白氨酸硫酸铜溶液 (取L 异白氨酸 1.3g、硫酸铜 1.0g和水 10 0 0ml溶解用 0 .1mol/L盐酸或 0 .1mol/L氢氧化钠调pH至 3.5 ) 甲醇 (75∶2 5 ) ;检测波长 :32 0nm。结果甲磺酸帕珠沙星右旋体在 0 .5～ 10 0 μg/ml浓度范围内呈良好的线性关系 (r=0 .9993) ,平均回收率为 99.5 4 % ,RSD为 1.0 1% (n =9)。结论此法快捷、专属性及重现性好 ,可用于甲磺酸帕珠沙星和D 甲磺酸帕珠沙星杂质的含量测定。     

反相高效液相色谱法测定兔血清中甲磺酸帕珠沙星浓度

目的:建立反相高效液相色谱法(RP-HPLC法)测定兔血清中甲磺酸帕珠沙星的浓度.方法:采用YWG C18色谱柱(4.6 mm×250 mm,5 μm),流动相为乙腈-0.5%磷酸溶液-三乙胺(55:44.5:0.5),流速为1.0 mL/min,进样量为20μL,检测波长为254nm,柱温为35℃,血清样品以诺氟沙星为内标.结果:甲磺酸帕珠沙星的线性范围为1～40μg/mL,最低检测浓度为0.1μg/mL,平均回收率在97.6%～106.1%之间,日内、日间RSD均小于5.0%.结论:RP-HPLC法精确、灵敏、稳定,可用于甲磺酸帕珠沙星血药浓度的测定和药代动力学研究.     

高效液相色谱法同时测定帕珠沙星和氨茶碱的含量

目的:建立同时测定帕珠沙星和氨茶碱含量的HPLC方法,并考察两种药物配伍后的稳定性。方法:分析柱为shimpackC18柱(150mm×4.6mm);流动相为磷酸二氢钾缓冲液-甲醇(17∶10),用磷酸调pH至3.7;检测波长为239nm。结果:帕珠沙星线性范围为0.5~5.0mg.L-1(r=0.9997)。相对回收率为101.4%;茶碱线性范围为1.0~20.0mg.L-1(r=0.9998)。相对回收率为100.2%。结论:以HPLC法用甲醇做溶剂可同时测定帕珠沙星与氨茶碱的含量。该方法简便、准确、灵敏。     

反相高效液相色谱法测定血浆中的帕珠沙星

目的:建立反相高效液相色谱法测定人血浆中帕珠沙星浓度,用于帕珠沙星人体药动学研究.方法:采用YMC C18(150 mm×4.6 mm,5 μm)色谱柱,柱温为35℃,流动相为乙腈-0.025 mol·L-1醋酸钠(醋酸调pH 2.6)(13:87),流速为1 mL·min-1.以盐酸芦氟沙星为内标,检测波长249 nm.结果:标准曲线线性范围78.125～2 000μg·mL-1;萃取回收率66.76%～72.76%;方法回收率97.85%～110.9%;日内RSD在5.1%～9.9%;日间RSD在4.8%～6.2%.结论:本方法快速、灵敏、准确、简便,适用于帕珠沙星血药浓度测定及药动学研究.     

甲磺酸帕珠沙星凝胶剂的制备与质量控制

目的：建立甲磺酸帕珠沙星凝胶剂的制备方法和质量标准。方法：以卡波姆为凝胶基质,制备甲磺酸帕珠沙星凝胶。采用高效液相色谱法测定凝胶中甲磺酸帕珠沙星的含量,色谱柱：Diamonsil C18（250mm×4．6mm,5um）;流动相：乙腈-磷酸三乙胺水溶液（含0．5％磷酸,1％三乙胺）（30：70）;流速：1．0ml·min^-1;检测波长：240nm;进样量：20ul。结果：甲磺酸帕珠沙星在10．54～52．7ug·ml^-1范围内有良好的线性关系,r=0．9993,平均回收率为99．67％,RSD=1．79％。结论：该制备工艺简单、易行,质量控制方法切实可行。     

HPLC测定人血浆中帕珠沙星浓度

目的建立测定人血浆中帕珠沙星浓度的高效液相色谱法。方法血浆样品用10%高氯酸沉淀蛋白。色谱柱为Diamonsil C18柱(200mm×4.6mm,5μm),流动相为0.02mol·L-1磷酸二氢钠溶液(含三乙胺0.5%,用磷酸调至pH3.0)-乙腈(82∶18),流速为1.0mL·min-1,紫外检测波长245nm。结果血浆中内源性物质对样品测定无干扰。本方法线性范围为0.05～50μg·mL-1(r=0.9999),最低定量浓度为0.05μg·mL-1,提取回收率大于80%,方法回收率为100.6%～101.4%,日内、日间RSD均小于6%。结论本法简便、灵敏、准确,适用于帕珠沙星药动学的研究。     

RP-HPLC法检测甲磺酸帕珠沙星注射剂中右旋体含量

目的 :建立RP HPLC法检测甲磺酸帕珠沙星注射剂中右旋体含量。方法 :采用岛津C1 8柱 (4 6mm× 2 5 0mm ,5 μm) ,流动相为甲醇 手性溶液 (30∶70 ) ,流速为 1 0mL min ,紫外检测波长为 32 0nm。 结果 :甲磺酸帕珠沙星右旋体的保留时间为 6 8min ,其浓度在 12 5 2～ 37 5 4 μg mL范围内 ,呈良好的线性关系 (r =0 9995 ,n =5 ) ,平均回收率为 99 16 % ,RSD为 0 33% (n =5 )。结论 :本法简便快速 ,精密度良好 ,可作为甲磺酸帕珠沙星制剂的质量控制方法。     

甲磺酸帕珠沙星乳膏剂的配制及质量控制

目的:建立甲磺酸帕珠沙星乳膏剂的制备方法和质量标准.方法:采用反相高效液相色谱法(RP-HPLC法)测定甲磺酸帕珠沙星的含量,以zorbax C18柱为色谱柱(4.6 mm×250 mm,10μm),流动相为磷酸盐缓冲液-甲醇-三乙胺(50:49.5:0.5),流速为1.0 mL/min,进样量为20μL,检测波长为254 nm.结果:RP-HPLC法能很好分离被测组分与基质,线性范围为5～250μg(r=0.999 3),平均回收率为100.37%,RSD为1.48%.结论:该制备工艺简单,质量控制方法切实可行.     

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.