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。     

苯磺酸氨氯地平胶囊的高效液相色谱法测定

目的:建立高效液相色谱法测定苯磺酸氨氯地平胶囊含量,为质量控制提供有效的分析手段.方法:色谱柱:Phenomenex ODS C18( 5μm、4.6mm ×150mm);流动相:甲醇-0.03mol·L-1磷酸二氢钾溶液(65:35);检测波长:2 39nm.结果:制剂中辅料和有关物质对主药无干扰,苯磺酸氨氯地平在浓度9.952～99.520μg·ml-1范围内线性关系良好,相关系数r＝0.9999(n=6);平均回收率分别为99.09%、100.4%、101.2%,RSD为0.12%.结论:本法专属性好,准确,简便.杂质,可有效控制本品质量.     

苯磺酸氨氯地平片的质量控制研究

目的:针对苯磺酸氨氯地平有显著降压效果,建立苯磺酸氨氯地平片的质量控制研究,为复方质量控制标准提供依据。方法:采用高效液相色谱(HPLC)法测定苯磺酸氨氯地平的含量。色谱柱:Phenomenex C18柱(200 mm×4.6 mm,5μm);流动相:0.03 mol.L-1KH2PO4-甲醇(25∶75);检测波长:237 nm;流速:1 mL.min-1;柱温:室温。采用浆法测定溶出度,并计算累计溶出百分率。结果:苯磺酸氨氯地平在10～70μg.mL-1的浓度范围内与峰面积线形良好,线性回归方程为:Y=18 914 X+13 640,相关系数为r=0.999 3;平均回收率为100.65%,RSD为0.99%;溶出时间为30 min时累积释放百分率达80%,符合《中华人民共和国药典》规定。结论:各项检验方法简便、准确、可靠,可作为该制剂的质量控制方法。     

HPLC测定复方苯磺酸氨氯地平胶囊的含量

目的 采用HPLC法测定复方苯磺酸氨氯地平胶囊的含量.方法 采用Diamonsil C18色谱柱(150 mm×4.6 mm,5μm),流动相为甲醇-0.03 mol·L-1磷酸二氢钾溶液(75∶25),流速1.0 mL·min-1,检测波长238 nm.结果 苯磺酸左旋氨氯地平0.25～500 μg·mL-1与峰面积的线性关系良好(r=0.9999),平均回收率为99.6%(RSD=0.7%);辛伐他汀5.0μg·mL-1～1.0 mg·mL-1与峰面积的线性关系良好(r=0.9999),平均回收率为99.9%(RSD=0.6%).结论 所建方法准确、简便、快速,可用作复方苯磺酸氨氯地平胶囊的含量测定方法.     

HPLC法测定复方盐酸贝那普利片中盐酸贝那普利和苯磺酸氨氯地平的含量

目的建立复方盐酸贝那普利片中盐酸贝那普利和苯磺酸氨氯地平含量测定的HPLC法。方法采用Diamonsil C18柱(200 mm×4.6 mm,5μm);流动相为氯化钾溶液(1 000 mL中含90 mmoL氯化钾和10 mmoL盐酸,pH值2.06)-水-甲醇(体积比为17∶25∶58),每1 000 mL流动相中加入612 mg高氯酸钠;流速为1 mL.min-1;检测波长为240 nm;柱温为35℃;进样量为20μL。结果盐酸贝那普利与苯磺酸氨氯地平可达到较好分离,盐酸贝那普利的质量浓度在10.0～200.0mg.L-1内与峰面积呈良好的线性关系(r=0.999 8);苯磺酸氨氯地平(按氨氯地平计)质量浓度在5～100 mg.L-1内与峰面积呈良好的线性关系(r=0.999 8)。盐酸贝那普利与苯磺酸氨氯地平的平均回收率分别为99.9%(n=9)和100.4%(n=9)。结论 HPLC法适用于复方盐酸贝那普利片中盐酸贝那普利和苯磺酸氨氯地平的含量测定。     

苯磺酸氨氯地平片两种含量测定方法比较<中文作者一>=刘放

目的 采用高效液相色谱法和紫外分光光度法同时测定苯磺酸氨氯地平片的含量,为质量控制提供有效的分析手段.方法 高效液相色谱法:色谱柱:DI AMONSIL C18(4.6mm×250mm,5μm);流动相:甲醇-0.03mol·L-1磷酸二氢钾水溶液(75∶25);检测波长:237nm.紫外分光光度法:检测波长:365nm.结果 高效液相色谱法:制剂中其它成分不干扰测定,氨氯地平峰和杂质峰达到有效分离.氨氯地平浓度在15.28~33.61μg·mL-1范围内线性关系良好(r=0.9994,n=7),平均回收率为99.79%~100.21%,RSD为0.33%~1.11%.紫外分光光度法:氨氯地平浓度在5.1~45.9μg·mL-1浓度范围内具有良好的线性关系(r=0.9997,n=9),平均回收率为96.65%~98.13%,RSD为0.55%~1.32%.结论 两种方法均可用作苯磺酸氨氯地平片剂的质量控制.     

HPLC法测定小儿氨酚匹林咖啡因片中四种成分的含量

目的:建立HPLC法同时测定小儿氨酚匹林咖啡因片中对乙酰氨基酚、咖啡因、阿司匹林及水杨酸的含量.方法:采用岛津ODS-VP色谱柱(4.6 mm×150 mm,5μm);以甲醇-0.01mol·L-1磷酸溶液(30:70)(用三乙胺调节pH值至3.1)为流动相;检测波长为220nm;流速为1.0 mL·min-1.结果:在建立的色谱条件下,对乙酰氨基酚、咖啡因、阿司匹林、水杨酸的线性范围分别为12.6～126 nag·L-1(r=0.999 9);3.0～30.0 rag·L-1(r=1.000 0);23.0～230 mg·L-1(r=0.999 8);0.115～6.9 mg·L-1(r=1.000 0).对乙酰氨基酚、咖啡因、阿司匹林的平均回收率分别为99,1%(RSD=1.32%,n=9);100.0%(RSD=0.57%,m=9);99.0%(RSD=1.09%,n=9).结论:本法简便、快捷,准确度高,专属性强,重现性好,可用于小儿氨酚匹林咖啡因片中对乙酰氨基酚、咖啡因、阿司匹林的含量测定及水杨酸的限度控制.     

餐时血糖调节剂米格列奈钙的RP-HPLC法人肝微粒体药物浓度测定

目的:建立人肝微粒体中米格列奈的高效液相色谱测定法.方法:采用Diamonsil-C18色谱柱(200 mm×4.6 mm,5μm);流动相为乙腈-0.02 mol·L-1KH2PO4缓冲液(pH 4.0)(43:57);流速为1.0 mL·min-1;紫外检测波长为210 nm;进样量为20 mL.结果:米格列奈最低检测限为2 μmol·L-1;线性范围为5～1 000 μmol·L-1(r=0.999 9);最低定量浓度为5μmol·L-1(RSD<5%,n=5);低、中、高3种浓度日内、日间RSD(n=5)分别为1.9%,1.6%,1.4%和3.8%,4.0%,3.8%;绝对回收率平均为94.4%,相对回收率平均为101.2%.结论:本实验建立的人肝微粒体中米格列奈的高效液相测定方法操作简便、结果准确.     

高效液相色谱法测定人血浆中氨溴索含量

目的:建立测定人血浆中氨溴索的高效液相色谱法。方法:色谱柱为ZORBAX Eclipse XDB-C18(4.6mm×150mm,5μm);保护柱为Eclipse XDB-C18(4.6mm×12.5mm,5μm);流动相为乙腈-磷酸氢二胺缓冲液(pH7.0)(45∶55);紫外检测波长242nm;流速1.0mL.min-1;柱温30℃;内标为盐酸地尔硫卓。结果:回归方程线性良好,方程:A=0.0021C 0.029 5,r=0.9999(n=5),线性范围为10~640μg.L-1,最低检测质量浓度为5μg.L-1。低、中、高(20,160,480μg.L-1)3种质量浓度的绝对回收率和相对回收率分别为90.6%,85.6%,91.8%和102.4%,91.8%,93.3%。日内、日间RSD均小于10%。结论:该方法适用于测定人血浆中氨溴索含量,结果准确、可靠。     

高效液相色谱法测定雷贝拉唑钠肠溶胶囊的含量和有关物质

目的:采用高效液相色谱法建立雷贝拉唑钠肠溶胶囊有关物质检查及其含量测定方法。方法:Kromasil(4.6mm×250mm,5μm)色谱柱;柱温为20℃:流动相为0.05mol.L-1磷酸二氢钾缓冲溶液(0.1mol.L-1氢氧化钠溶液调pH7.0)-乙腈(70∶30);流速为1mL.min-1;测定波长为290nm。结果:雷贝拉唑钠在50～400mg.L-1范围内线性关系良好,r=0.9998(n=5);平均回收率为99.25%,RSD为2.08%(n=9)。结论:本方法简便,迅速,准确,可靠,专属性强。     

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.     

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.     

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.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

Abstract

The uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors.     

Alzheimer’s disease – current trends in basic and clinical research. Highlights from the 16th ECNP

Advances in the molecular biological knowledge of neuronal nicotinic acetylcholine receptors (nAChRs) have led to a growing interest by the pharmaceutical industry in the development of novel compounds that selectively modulate nAChR function. The ability of (-)-nicotine, an activator of nAChRs, to enhance attentional aspects of cognition in animals and humans, to exert neuroprotective and anxiolytic-like effects, and presumably to mediate the negative correlation between smoking and Alzheimer's (and Parkinson's) Disease, has focused interest on the potential therapeutic utility of modulators of nAChR function for treatment of some of the deficits associated with these progressive, neurodegenerative conditions. Numerous compounds are known which activate nAChRs and which might serve as lead compounds toward the development of such agents. The pharmacologic diversity of neuronal nAChR subtypes suggests the possibility of developing selective compounds which would have more favourable side-effect profiles than existing agents. This broader class of agents, collectively called cholinergic channel modulators (ChCMs), is anticipated to encompass compounds which would have more favourable side-effect profiles than existing agents, which generally exhibit low selectivity. This selectivity may be achieved by preferentially activating some subtypes of nAChRs (i.e., Cholinergic Channel Activators, ChCAs) or inhibiting the function of other subtypes (Cholinergic Channel Inhibitors, ChCIs). An overview of the biology of nAChRs and the rationale for the use of ChCMs for the treatment of dementia related to neurodegenerative diseases are presented, followed by a discussion of lead compounds and compounds under consideration for clinical evaluation.