HPLC法测定替硝唑芬布芬胶囊中替硝唑和芬布芬的含量

建立替硝唑芬布芬胶囊含量测定的方法。采用高效液相色谱法,色谱柱:Throm C18;流动相:甲醇-乙腈-水(40∶60∶40)(调pH至3.0);流速:0.8ml.min-1;柱温:室温;检测波长:300nm。替硝唑和芬布芬在40.00~160.0μg.ml-1(r=0.9999)及15.00~60.00μg.ml-1(r=0.9998)的范围内,峰面积与浓度呈良好的线性关系;替硝唑与芬布芬的平均回收率分别为99.7%(RSD为0.7%)和99.8%(RSD为0.9%)。所建立的HPLC方法灵敏、专一、准确,可作为替硝唑芬布芬胶囊含量测定的方法。     

人体内阿昔洛韦血药浓度的HPLC测定

目的:建立阿昔洛韦血药浓度测定方法,用于阿昔洛韦缓释片血药浓度研究。方法:采用高效液相色谱法。分析柱为C1 8柱,流动相为2 %乙腈水溶液(p H3) ,检测波长2 5 4 nm。结果:样品组分在0 .0 5～1.0μg·ml- 1 线性良好(0 .9997) ,最低血浆药物检测浓度为0 .0 1μg·ml- 1。回收率为92 .36 %～99.2 1% ,日内及日间RSD<10 %。结论:本法简便、迅速、灵敏、准确,适合于临床药学研究需要。     

HPLC法测定人血浆中替硝唑的浓度

目的建立测定人血浆中替硝唑浓度的HPLC法。方法采用Diamomil C_(18)(200 mm×4.6 mm,5μm)色谱柱;流动相为乙腈-水(20:80,V/V);流速1.0 mL·min~(-1);检测波长310 nm;内标为甲硝唑。结果替硝唑血药浓度在0.5～50mg·L~(-1)内线性关系良好(r=0.9990);替硝唑低、中、高3种浓度的方法回收率为94.89%～99.53%,提取回收率为89.55%～95.60%,日内RSD<2%(n=5),日间RSD<5%(n=5)。结论本方法操作简便,准确可靠,可用于替硝唑临床血药浓度监测和药动学研究。     

固相萃取-高效液相色谱法测定人血浆中的替硝唑浓度

目的建立固相萃取结合高效液相色谱法测定人血浆中替硝唑浓度的方法。方法血浆样品经C18固相萃取小柱净化后进样。色谱柱:HyperS il C18柱(250 mm×4.6 mm,5μm),流动相:磷酸二氢钾(含0.1%三乙胺,磷酸调pH=3.2)-乙腈(89∶11),柱温:25℃,流速:1 m L/min,检测波长:236 nm,进样量:30μL。结果替硝唑血药浓度在0.5~50 mg/L之间呈良好线性关系(r=0.999 5),线形方程Y=1.012 C-0.053 1,相对标准偏差<5%,回收率>90%。结论该方法操作简便、准确可靠,灵敏度高,适用于替硝唑的血药浓度检测。     

HPLC法测定人血浆中替硝唑的浓度

目的采用HPLC法测定人血浆中替硝唑的浓度。方法以D iam onsilTMC18反相柱(250 mm×4.6 mm,5μm)为色谱柱,流动相为甲醇-0.03 m o l.L-1醋酸铵(25∶75,V/V),流速0.8 mL.m i-n 1,紫外检测波长320 nm,以乙酸乙酯∶二氯甲烷(4∶1,V/V)为提取剂。结果替硝唑的高、中、低3种浓度的回收率分别为111.01%、99.00%和100.74%,日内RSD≤5.87%(n=5)、日间RSD≤7.82%(n=3);线性范围为0.25~75 m g.L-1,回归方程为:c=25.65F-0.03,r=0.9998(n=9);最低检测浓度为0.05 m g.L-1(R sn≥3)。结论该方法可用于临床血药浓度监测和药动学研究。     

高效液相色谱法测定替硝唑的含量

目的建立替硝唑的含量测定方法.方法采用高效液相色谱法,色谱柱为DiamonsilTM C18(5μm,250 mm×4.6 mm),以甲醇-水-冰醋酸(20:80:0.5)为流动相,检测波长310 nm,流速1.0 ml/min.结果替硝唑在0.2404～2.404μgμg范围内呈良好的线性关系,r=0.9998;平均回收率为99.8%,RSD为0.3%.结论本法专属性强,灵敏度高,准确性好.     

高效液相色谱法测定人血浆中加替沙星浓度

目的:建立HPLC法测定人血浆中加替沙星浓度的方法。方法:采用噻克硝唑为内标,色谱柱为Polaris C18-A柱(150*4.6mm),流动相为乙腈:0.05M的枸缘酸溶液(22:78),流速1.0ml/min,检测波长为295nm。结果:加替沙星血清浓度在0.015～6.48μg·ml-1范内具有良好线性关系,最低定量限为0.015μg·ml-1,方法回收率为99.1%～101.0%,日内、日间RSD均<7%。结论:本法简便、准确、灵敏,适用于加替沙星血药浓度监测及人体药代动力学研究。     

高效液相色谱法测定复方呋已栓三主药的含量

目的建立高效液相色谱法测定复方呋已栓中替硝唑、已烯雌酚和呋喃西林含量的方法。方法用Hypersil C18(250mm×4.6mm,5μm)色谱柱;以甲醇-水-乙醚(30:70:1)为流动相;流速为1.0mL.min-1;柱温为20℃;检测波长为263nm。结果替硝唑、已烯雌酚和呋喃西林的保留时间分别为4.23,5.42,6.35min,理论塔板数分别为5320,2450和3560;HPLC法测定的线性范围分别在192.1～448.1μg.mL-1(r氯=0.9999),5.8～17.2μg.mL-1(r乙=0.9995)和9.7～22.6μg.mL-1(r呋=0.9998);平均回收率分别为100.4%,99.99%和101.5%,RSD分别为1.2%(n=5),0.576%(n=5)和1.8%(n=5);该法的精密度和稳定性良好。结论本法用于复方呋已栓中替硝唑、呋喃西林和已烯雌酚的含量测定简便、快速、准确、可靠。     

SPE-HPLC测定索他洛尔血药浓度

目的:建立检测索他洛尔血药浓度的SPE-HPLC方法.方法:以C18固相萃取小柱预处理样品.色谱柱为Shim-pack VP-ODS C18柱,流动相为乙腈-水-三乙胺(5:95:0.2,v/v,磷酸调pH4.0),流速0.8 ml·min-1,柱温30℃,检测波长为227 nm,进样量20μl.结果:索他洛尔在0.04～5.0μg·ml-1浓度范围内线性关系良好,回归方程为Y=1.79X-0.02,r=0.999 8,索他洛尔萃取回收率为91.05%～100.75%,方法回收率为98.55%～101.36%(n=5),日内RSD小于5%,日间RSD小于10%.结论:本方法灵敏、准确,可用于索他洛尔的血药浓度检测.     

RP-HPLC法同时测定壳聚糖止血海绵中3组分的含量

目的:建立壳聚糖止血海绵中地塞米松磷酸钠、替硝唑及克林霉素的RP-HPLC含量测定方法。方法:色谱柱为Dis- covery C18柱(150 mm×4．6 mm,5μm);流动相为乙腈-0．05 mol·L-1磷酸二氢钾缓冲液-三乙胺(35:65:0．3),用磷酸调pH至5．3;流速1．0 ml·min-1;检测波长210 nm。结果:地塞米松磷酸钠、替硝唑、克林霉素分别在2-10μg·ml-1(r=0．999 7)、6 -30μg·ml-1(r=0．999 8)、30-150μg·ml-1(r=0．999 8)线性范围内呈现良好的线性关系。3组分的平均回收率分别为99．4％(RSD=2．1％);98．7％(RSD=1．7％)、99．2％(RSD=1．9％)。结论:本法操作简便、快速、结果准确。可作为该制剂的质控方法。     

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.