HPLC法测定祛湿止痒搽剂中大黄素的含量

目的采用高效液相色谱法测定祛湿止痒搽剂中大黄素的含量。方法采用Shim-packclc-ODS柱,以甲醇-0·1%磷酸溶液(85∶15)为流动相,测定波长:288nm。结果大黄素的线性范围为0·92~9·20μg·ml-1(r=0·9999),平均回收率为99·2%(RSD=3·40%,n=5)。结论该方法准确、可靠、重复性好,可作为祛湿止痒搽剂质量控制方法。     

高效液相色谱法测定盐酸阿莫罗芬搽剂的含量

摘要：目的:建立盐酸阿莫罗芬搽剂的含量测定方法。方法:利用HPLC技术,采用Alltima C18色谱柱(150 mm×4.6 mm, 5μm),流动相为甲醇-0.02 mol·L-1磷酸二氢钾溶液(磷酸调pH至3.0)(75∶25),流速为1.0 ml·min-1,检测波长为214 nm,柱温为30℃,进样体积为10μl。结果:盐酸阿莫罗芬在50.42～151.3μg·ml-1与峰面积呈良好的线性关系(r=0.999 9);平均回收率为99.30%,RSD为0.78%(n=9)。结论:该方法准确、简单、快速,能够用于盐酸阿莫罗芬搽剂的含量测定。     

HPLC法测定氯霉素地塞米松搽剂的含量

目的:建立HPLC法测定氯霉素地塞米松搽剂中氯霉素和醋酸地塞米松的含量。方法:色谱柱为C18柱(4.6mm×250mm,5μm),流动相为甲醇-水(68∶32),流速为1.0ml·min-1,检测波长为240nm。结果:氯霉素在400~1200μg·ml-1(r=1.000)范围内线性关系良好,平均回收率为100.1%(n=9),RSD为0.32%;醋酸地塞米松在10~30μg·ml-1(r=1.000)范围内线性关系良好,平均回收率为100.8%(n=9),RSD为0.71%。结论:该方法简便、准确、快速,可同时测定两组分的含量。     

比色法测定痤疮搽剂中甲硝唑和氯霉素的含量

目的:建立比色法测定痤疮搽剂中的甲硝唑和氯霉素的含量方法.方法:用显色剂N-(1-荼基)乙二胺盐酸盐,经不同处理,分别比色测定痤疮搽剂中的甲硝唑和氯霉毒的含量.结果:甲硝唑在1-6μg·ml-1的浓度范围内呈良好的线性(γ=0.9999).平均回收率为99.5%,RSD为0.43%;氯霉素在1-5μg·ml-1的范围内呈良好的线性(γ=0.9999).平均回收率为99.6%,RSD为0.54%.结论:本法可用于该制剂的测定,操作简便,结果准确,灵敏度高.     

高效液相色谱法测定复方地塞米松搽剂中盐酸达克罗宁的含量分析

目的建立采用高效液相色谱法测定复方地塞米松搽剂中盐酸达克罗宁的含量的方法。方法采用Kromasil C18柱(4.6mm×250mm,5μm),HPLC反相法进行分离,紫外检测器检测,流动相为乙腈-水-冰醋酸-三乙胺(45∶55∶0.5∶0.5);流速:1.5mL·min-1;测定波长:279nm;柱温:40℃:进样:20μL。结果该方法没有受到处方中基质干扰。盐酸达克罗宁的线性范围为0.1003～0.7021μg(r=0.9998,n=6),平均回收率分别为98.8%,RSD为0.97%(n=9)。结论该方法操作简便、准确、快速、重现性好,可用于复方地塞米松搽剂中盐酸达克罗宁的含量测定。     

HPLC法同时测定复方水杨酸搽剂中乳酸依沙吖啶与水杨酸的含量

目的建立同时测定复方水杨酸搽剂中乳酸依沙吖啶和水杨酸含量的HPLC法。方法采用Alltima C18色谱柱(150mm×4.6mm,5μm);以甲醇-1mL·L~(-1)磷酸(50∶50)为流动相;流速:1.0mL·min~(-1);检测波长:270nm。结果乳酸依沙吖啶和水杨酸的线性关系良好,线性相关系数(r)分别为1.000 0和0.999 0;精密度和稳定性良好,RSD值均小于1.0%;回收率良好,乳酸依沙吖啶和水杨酸的平均回收率(n=9)分别为100.8%和101.3%。结论该方法准确、简单、快速,可用于同时测定复方水杨酸搽剂中乳酸依沙吖啶和水杨酸的含量。     

复方地塞米松搽剂的制备及质量控制

目的:制备复方地塞米松搽剂并建立其质量控制方法。方法:以氮酮为促透剂、乙醇为溶剂制备复方地塞米松搽剂,采用高效液相色谱法测定制剂中主药醋酸地塞米松和维生素E的含量。结果:醋酸地塞米松、维生素E检测浓度分别在2~40μg/ml、80~800μg/ml范围内呈良好线性关系,平均回收率分别为100·5%(RSD=0·82%)、98·6%(RSD=0·59%)。结论:该制剂处方合理,质量控制方法简便、准确。     

高效液相色谱法测定克拉维丁搽剂中醋酸地塞米松含量

目的测定克拉维丁搽剂中醋酸地塞米松的含量。方法用高效液相色谱法,色谱柱为C18柱(150 mm×4.6mm,5μm);流动相为甲醇-水-冰醋酸(80200.5);检测波长为240nm;进样量20μl;柱温30℃;流速1ml/min。结果醋酸地塞米松在2.00~64.00μg/ml范围内线性关系良好,Y=0.405 2 X+0.804 2(r=0.999 9),平均回收率为99.3%,RSD=0.93%(n=9)。结论该法便捷,重现性好,适用于克拉维丁搽剂中醋酸地塞米松的含量测定。     

高效液相色谱法测定氯霉素地塞米松搽剂中二组份的含量

目的建立一种快速、准确的高效液相色谱法测定氯霉素地塞米松搽剂中的氯霉素和醋酸地塞米松含量的方法。方法色谱柱岛津VP-ODS(5μm,150mm×4.6mm)流动相:甲醇-水(70∶30);流速:1mL.m in-1;检测波长:240nm;柱温:室温;进样量:20μL。结果氯霉素进样量在5.00μg~30.00μg范围内线性良好,r=0.99999。平均回收率为99.70%,RSD=0.68%(n=9);醋酸地塞米松进样量在0.13μg~0.75μg范围内线性良好,r=0.99999。平均回收率为99.97%,RSD=1.38%(n=9)结论试验结果表明本法简便快速,重现性好,结果准确可靠,可以作为氯霉素地塞米松搽剂中氯霉素和醋酸地塞米松含量测定的方法。     

HPLC法测定醋酸地塞米松搽剂中醋酸地塞米松的含量

目的建立高效液相色谱法测定醋酸地塞米松搽剂中醋酸地塞米松的含量.方法采用Agilent高效液相色谱仪,流动相为乙腈-水(40∶60),流速1.5mL·min-1,检测波长240 nm,柱温:35℃.结果醋酸地塞米松在7.812～85.932μg·mL-1范围内,线性关系良好,r=0.999 9,回收率为99.3%.结论本法可准确测定醋酸地塞米松搽剂中醋酸地塞米松的含量,适用于产品的质量控制.     

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.     

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.     

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.     

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.