反相HPLC法测定盐酸非索非那定片的含量及有关物质

目的建立反相HPLC法测定盐酸非索非那定片的有关物质及含量。方法采用安捷伦公司HP1100、HP1200高效液相色谱仪;Krom asil C18柱(5μm,250 mm×4.6 mm);流动相:磷酸盐缓冲液[磷酸二氢钠7.8 g,辛烷磺酸钠2.16 g,加水至1 000m l,用磷酸调节pH值至3.0]-乙腈(60∶40);流速:1.0 m l·m in-1;检测波长:220 nm;柱温:30℃,进样:20μl。结果盐酸非索非那定在60~180 mg·L-1浓度范围线性关系良好(r=0.999 9),最低检测限0.9 ng,方法精密度RSD=0.47%,各杂质峰与主峰分离良好。结论该方法简单方便专属性强,准确可靠,可用于测定盐酸非索非那定片的含量及有关物质。     

高效液相色谱法测定复方磷酸哌喹片中磷酸哌喹和磺胺多辛的含量

目的:建立同时测定复方磷酸哌喹片中磷酸哌喹和磺胺多辛含量的方法。方法:采用高效液相色谱法,色谱柱为Waters Atlantis C18(250 mm×4.6 mm,5μm),以10 mmol.L-1庚烷磺酸钠与25 mmol.L-1磷酸二氢钾等量混合溶液-乙腈-甲醇(53∶16∶31)(用磷酸调节pH至2.5)为流动相,流速:0.9 mL.min-1,检测波长:254 nm,柱温:40℃,进样量:10μL。结果:磷酸哌喹和磺胺多辛分别在26.39～263.90μg.mL-1和5.128～51.28μg.mL-1范围内线性关系良好;磷酸哌喹平均回收率为99.28%(RSD为0.90%),磺胺多辛平均回收率为100.13%(RSD为1.33%)。结论:该方法快速、结果准确可靠,适用于复方磷酸哌喹片的含量测定。     

高效液相色谱法测定恩他卡朋片的含量

目的建立恩他卡朋片含量测定的方法。方法色谱柱:Intersil C18(4.6 mm×250 mm,5μm),流动相:甲醇-乙腈-0.03 mmol.L-1磷酸二氢钾缓冲溶液(磷酸调节pH至2.75)(35∶25∶40,V/V/V),检测波长:310 nm,柱温:30℃,流速:1.0 mL.min-1。结果恩他卡朋的线性范围为10～50 mg.L-1(r=0.999 9),平均回收率为(99.74±0.69)%,RSD=0.68%(n=9)。结论本方法简便、准确、重现性好,可用于恩他卡朋片的含量测定。     

高效液相色谱法测定氯强油搽剂中氯霉素和醋酸泼尼松的含量

目的:建立高效液相色谱法测定氯强油搽剂中氯霉素和醋酸泼尼松的含量。方法:测定氯霉素含量用Spherisorb C18柱(4.6mm×250mm,5μm),流动相为甲醇-0.02mol.L-1磷酸二氢钾(用磷酸调pH至3.0)(60∶40,v/v),流速为0.9mL.min-1,检测波长为242nm;测定醋酸泼尼松含量用C18色谱柱(4.6mm×250mm,5μm),以甲醇-水(60∶40,v/v)为流动相,检测波长为240nm,流速为1.0mL.min-1。结果:氯霉素在100.1~500.4mg.L-1范围内线性关系良好(r=0.999 6),平均回收率为100.2%;醋酸泼尼松在10~150mg.L-1范围内线性关系良好,峰面积积分值与浓度呈良好线性关系(r=0.999 6);平均回收率为99.4%(RSD=1.7%)。结论:高效液相色谱法可以用于该制剂得含量测定和质量控制,方法简便、灵敏、结果准确。     

高效液相色谱法测定苯磺酸氨氯地平片的含量及有关物质

目的:建立高效液相色谱法测定苯磺酸氨氯地平片的含量及有关物质的方法。方法:色谱柱为:Hypersil ODS2(4.6mm×250mm,5μm);柱温为25℃;检测波长为237nm;流动相为甲醇-0.03mol.L-1磷酸二氢钾水溶液(70∶30);流速为1mL.min-1。结果:制剂中其它成分不干扰测定,杂质峰和主峰达到有效分离。苯磺酸氨氯地平溶液在8.9~71.2mg.L-1范围内线性关系良好(r=0.999 9,n=5),平均回收率为99.9%,RSD为1.0%。结论:该方法适用于测定苯磺酸氨氯地平片的含量及其有关物质,方法简单,结果准确,专属性强。     

HPLC法测定枸橼酸喷托维林片的含量

目的建立高效液相色谱法测定枸橼酸喷托维林片的含量。方法采用KromasilODS色谱柱(250mm×4.6mm,5μm);流动相:0.05mol.L-1枸橼酸-乙腈-三乙胺(55∶45∶0.05),用冰醋酸调pH7.5;流速:1.0mL.min-1;检测波长:230nm。结果枸橼酸喷托维林的质量浓度在500～1500mg.L-1范围内与峰面积呈良好的线性关系,r=0.9998,平均回收率为99.8%,RSD为0.21%(n=6)。结论方法专属性强,重现性好,操作简便,结果准确,可用于枸橼酸喷托维林片的含量测定。     

至宝三鞭丸中马钱苷的含量测定

目的建立RP-HPLC法测定至宝三鞭丸中马钱苷的含量。方法采用RP-HPLC法。色谱柱:C18柱(250 mm×4.6 mm,5μm);流动相:四氢呋喃-乙腈-甲醇-0.5 g.L-1磷酸溶液(1∶8∶4∶48);检测波长:236 nm;流速:1.0 mL.min-1;柱温:40℃。结果马钱苷在0.018 5~0.738μg范围内与峰面积呈良好的线性关系(r=0.998 4),该制剂中马钱苷的平均回收率为99.7%,RSD为0.52%(n=5)。结论该方法简便,结果准确、可靠,可用于至宝三鞭丸中马钱苷的含量测定。     

RP-HPLC法测定PAC-1盐酸盐的含量及有关物质

目的建立RP-HPLC方法测定PAC-1盐酸盐含量并进行有关物质检查。方法采用KromasilC18色谱柱(150 mm×4.6 mm,5μm),流动相:乙腈-甲醇-磷酸盐缓冲液(30 mmo.lL-1磷酸二氢钾,体积分数为0.06%的磷酸溶液)(体积比为35∶5∶60),流速:1.0 mL.min-1,UV检测波长:281 nm,柱温:35℃。结果PAC-1盐酸盐在2.00~50.10 mg.L-1内线性关系良好(r=0.999 9),平均回收率为100.3%(RSD=0.8%)。PAC-1盐酸盐与其有关物质得到良好分离,检测限为0.2 ng。结论本方法可用作PAC-1盐酸盐含量测定和有关物质检查。     

反相高效液相色谱法测定醋酸去氨加压素片及注射液含量

目的:建立反相高效液相色谱法测定醋酸去氨加压素片及醋酸去氨加压素注射液含量。方法:选用Kromasil C18柱(4.6 mm×250 mm,5μm);流动相:乙腈-水(20∶80)(含0.067 mol.L-1磷酸二氢钾,0.067 mol.L-1磷酸氢二钠,调节磷酸盐比例使pH为7.0);流速:1.0 mL.min-1;紫外检测波长:220 nm;进样量:片剂20μL,注射剂100μL;柱温:室温。结果:方法的线性范围为0.008～2μg,r=0.9999,最低检测限为4.0 ng;片剂的平均回收率为101.2%,RSD为0.78%(n=9),注射液的平均回收率为100.8%,RSD为1.1%(n=9)。结论:本方法快速灵敏,结果准确可靠,可用于醋酸去氨加压素片及醋酸去氨加压素注射液含量的测定。     

HPLC法测定兰索拉唑片含量及有关物质

建立高效液相色谱法测定兰索拉唑片含量及有关物质的方法。方法采用C18色谱柱(4.6mm×250mm,5μm),以水-乙睛-三乙胺(60∶40∶1)用磷酸调pH7.0为流动相,流速:1.0mL.min-1,检测波长为285nm,进样量20μL,柱温35℃。结果兰索拉唑浓度在19.76~177.84μg.mL-1时,其峰面积与浓度的线性关系良好(r=1);平均回收率为99.6%,平均相对标准偏差RSD为0.5%;检测限为0.02ng.mL-1。结论本法快速、简便、准确,灵敏度高,适用于兰索拉唑片含量及有关物质测定。     

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.