用反相高效液相色谱法测定复方头孢氨苄胶囊中头孢氨苄和甲氧苄啶的含量

建立一种用反相高效液相色谱法检测复方制剂中头孢氨苄和甲氧苄啶含量的方法 .头孢氨苄浓度为 0 .0 5～ 2 .0 0mg/mL、甲氧苄啶浓度为 0 .0 1～ 0 .40mg/mL时存在良好的线性关系 .头孢氨苄回收率为 10 0 .4% ,RSD =0 .5 8% (n =7) ;甲氧苄啶回收率为 10 0 .2 % ,RSD =0 .6 2 % (n =7) .     

双波长与一阶导数分光光度法联用测定复方头孢氨苄胶囊中头孢氨苄与TMP含量

目的:建立紫外可见分光光度法同时测定头孢氨苄/甲氧苄啶的方法。方法:应用双波长法,选择甲氧苄啶的等吸收点262nm、284nm为头孢氨苄的测定波长;应用一阶导数光谱法,以234nm(谷)处的半振幅为甲氧苄啶定量依据,消除头孢氨苄的干扰。结果:头孢氨苄的线性范围10~95μg/ml,甲氧苄啶 2~40μg/ml,平均回收率分别为 99.95%和 100.13%。二者日内、日间精密度的RSD均小于2%。结论:本方法快速、简便、结果准确,可作为复方头孢氨苄胶囊的含量测定。     

复方头孢氨苄片头孢氨苄甲氧苄啶含量测定方法改进

目的建立可同时测定复方头孢氨苄甲氧苄啶片中头孢氨苄与甲氧苄啶含量的高效液相色谱法。方法色谱柱为C18柱(250 mm×4.6 mm,5μm),以水-3.86%醋酸钠溶液-4%醋酸溶液-甲醇(742∶15∶3∶240)为流动相,流速1.0 mL/min,检测波长为235 nm。结果头孢氨苄进样量在6～119.9μg、甲氧苄啶进样量在1.20～24.0μg范围内与峰面积呈良好线性关系;头孢氨苄平均回收率为99.89%,RSD为0.28%;甲氧苄啶平均回收率为99.90%,RSD为0.85%。结论该方法便捷、专属性强,可用于样品的质量检查。     

双波长与一阶导数分光光度法联用测定复方头孢氨苄胶囊中头孢氨苄与TMP含量

建立紫外可见光光度法同时测定头孢氨苄/甲氧苄啶的方法。方法：应用双波长法,选择甲氧苄啶的等吸收点262nm、284nm为头孢氨苄的测定波长;应用一阶导数光谱法,以234nm(谷）处的半振幅为甲氧苄啶定量依据,消除头孢氨苄的干扰。结果：头孢氨苄的线性范围10～95ug/ml,甲氧苄啶2～40ug/ml,平均回收率分别为99.95%和100.13%。二者日内、日间精密度的RSD均小于2%。结论：本方法快速、简便、结果准确,可作为复方头孢氨苄胶囊的含量测定     

高效液相色谱法测定头孢氨苄甲氧苄啶胶囊的含量均匀度

目的建立头孢氨苄甲氧苄啶胶囊含量均匀度的测定方法。方法以0.025 mol/L磷酸溶液（用20%氢氧化钠调节pH至3.0）-乙腈（85∶15）为流动相,流速1 mL/min,检测波长235 nm,用高效液相色谱法测定含量。结果头孢氨苄质量浓度在12.5～125μg/mL、甲氧苄啶质量浓度在2.5～25μg/mL范围内与峰面积线性关系良好,平均回收率分别为99.9%和99.8%,RSD分别为0.38%和0.95%（n=9）。结论所用方法简便快捷,能准确地测定产品的含量均匀度,可用于头孢氨苄甲氧苄啶胶囊的质量控制。     

HPLC法同时测定联磺甲氧苄啶片中三组份的含量

目的:研究HPLC法同时测定联磺甲氧苄啶片中磺胺甲噁唑、磺胺嘧啶和甲氧苄啶的含量。方法:采用高效液相色谱法,色谱柱为C18柱(4.6 mm×250 mm,5μm),以0.025 mol/L磷酸溶液-乙腈(80∶20)为流动相,检测波长为220 nm。结果:磺胺甲噁唑、磺胺嘧啶和甲氧苄啶的线性范围分别为40￣240μg/ml(r=0.9999)、40￣240μg/ml(r=0.9999)和16～96μg/ml(r=0.9995),回收率分别为100.4%(RSD=0.30%)、100.4%(RSD=0.21%)、101.7%(RSD=1.29%)。结论:该法快速、简便、重现性好。     

HPLC法测定头孢氨苄甲氧苄啶颗粒含量的方法改进

目的头孢氨苄甲氧苄啶颗粒是由头孢氨苄和甲氧苄啶组成的复方制剂,本实验用HPLC法同时测定其两种成分的含量。方法用十八烷基硅烷键合硅胶为填充剂,以0.025mol/L磷酸溶液-乙腈（80：20）为流动相,检测波长为235nm,流速为每分钟0.8ml,理论塔板数按头孢氨苄峰计数应不低于3000。结果头孢氨苄在10.00～50.00μg/ml,甲氧苄啶在2.00～10.00μg/ml范围内,峰面积与其浓度呈良好线性关系,头孢氨苄的加样平均回收率为99.43%,RSD为0.28%,甲氧苄啶的加样平均回收率为99.21%,RSD为0.61%。结论与原标准相比,所得的头孢氨苄,甲氧苄啶两种成分峰面积与其浓度呈良好线性关系,峰形对称,拖尾因子小,结果比较准确。     

高效液相色谱法测定小檗碱甲氧苄啶胶囊中甲氧苄啶含量

目的建立小檗碱甲氧苄啶胶囊中甲氧苄啶的含量测定方法。方法色谱柱为Agelent C18柱(250 mm×4.6 mm,5μm),以甲醇-水(60∶40)为流动相,流速为1.0 mL/min,检测波长为265 nm。结果甲氧苄啶进样量在0.5～1.5μg范围内与峰面积呈良好线性关系,r=0.999 8,平均回收率为98.41%,RSD=1.13%(n=9)。结论该法适用于小檗碱甲氧苄啶胶囊中甲氧苄啶的含量测定。     

高效毛细管电泳法同时测定血浆中头孢羟氨苄和甲氧苄啶的含量

采用毛细管区带电泳法(CZE)测定血浆中头孢羟氨苄、甲氧苄啶的含量。以20mmol/L硼砂(pH7.1)为背景电解质,35cm×75μm(i.d)未涂层毛细管为色谱柱,于267nm处检测,操作温度25℃,分离电压为20kV,采用峰面积外标法定量。头孢羟氨苄和甲氧苄啶的线性范围分别为0.4~4.0和0.25~4.0μg/ml,检出限分别为0.1和0.18μg/ml(S/N=3)。该方法测得头孢羟氨苄和甲氧苄啶的在低、中、高浓度下的回收率均在95%以上,迁移时间的RSD分别为0.43%、1.44%;峰面积的RSD分别为3.34%、4.0%,日内、日间精密度均符合方法学要求。该方法用量少,简便,快速,准确,适合于血药浓度的监测。     

HPLC测定复方头孢氨苄中的头孢氨苄和甲氧苄啶含量方法的改进

目的对HPLC测定复方头孢氨苄胶囊中的头孢氨苄和甲氧苄啶含量方法进行改进并与原药品标准规定的溶媒萃取法进行比较。方法以0.025mol/L的磷酸(用20%的NaOH调节pH=3.0)-乙腈(88∶12)为流动相,以ODSC18柱为色谱柱,柱温为40℃,流速为1.0ml/min,检测波长为235nm。结果头孢氨苄在10～150μg/ml(r=0.99996)、甲氧苄啶在2～30μg/ml(r=0.99996)的浓度范围内呈线性关系;平均回收率分别为99.94%、99.47%;RSD分别为0.5%、0.4%。HPLC法与溶媒萃取法所测含量较为接近。结论与溶媒法相比较,HPLC法操作简单、快速、准确、灵敏度较高且两个主成分的分离度高。     

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.