高效液相色谱法测定盐酸普萘洛尔片含量

目的:采用高效液相色谱法测定盐酸普萘洛尔片的含量.方法:Diamonsil C18柱(4.6 mm×150 mm,5μm)为分析柱,流动相为甲醇-0.02 mol·L-1磷酸二氢钾溶液(50:50),流速0.9 ml·min-1,检测波长290nm.结果:盐酸普萘洛尔在50.7～405.9μg·ml-1范围内呈良好的线性关系,r=0.999 9,平均回收率为99.2%,RSD=0.92%(n=9).结论:本方法简单、快速、结果可靠.     

HPLC测定注射用蒲公英冻干粉针剂中的绿原酸和咖啡酸

目的 建立HPLC测定注射用蒲公英粉针剂中绿原酸、咖啡酸含量的方法.方法 采用DikmatmC18柱(200 mm x4.6mm,5μm),流动相为乙腈-0.1%磷酸水溶液(17:83),流速为1.0 mL·min-1,检测波长为326 nm,柱温为30℃.结果 绿原酸浓度0.108～3.464 μg·mL-1与峰面积的线性关系良好(r=0.9998),平均加样回收率为99.68%(n=9);咖啡酸浓度0.114～3.648μg·mL-1与峰面积的线性关系良好(r=0.9999).平均加样回收率为98.73%(n=9).结论 所建方法灵敏、简便、准确、重复性好,可用于蒲公英冻干粉针剂中绿原酸、咖啡酸的含量测定.     

RP-HPLC法测定唑来膦酸的含量及其相关物质

目的:建立测定唑来膦酸的含量和有关物质的RP-HPLC法.方法:采用C18色谱柱(200mm×4.6mm,5μm),流动相为乙腈-8mmol·L-1的焦磷酸钠(含20mmol·L-1四丁基氢氧化铵,磷酸调pH至6.8)(6:100),流速为1.0mL·min-1,检测波长215nm,柱温30℃.结果:唑来膦酸在20～160μg·mL-1范围内线性关系良好,r=0.999 9.加样回收率为100.1%,RSD=0.5%(n=9).结论:该法操作简便、准确,为唑来膦酸提供了方便可靠的含量测定及其有关物质的检测方法.     

高效液相色谱法测定硫酸锌尿囊素滴眼液中尿囊素的含量

目的:建立测定硫酸锌尿囊素滴眼液中尿囊素含量的高效液相色谱方法.方法:采用KromasilC18柱(150 mm×4.6 mm,μm),流动相为0.03 mol·min-1的磷酸二氢钠溶液.甲醇(90:10),检测波长为224nm,流速为1.0 mL·min-1,外标法计算.结果:线性范围为50.6～1 518.0 mg·min-1(r=0.999 7,n=7),回收率为100.3%(RSD为1.51%,n=9).结论:此方法快速简便,辅料无干扰,适用于该制剂的含量测定.     

HPLC法测定氧氟沙星滴耳液的含量

目的:建立测定氧氟沙星滴耳液含量的HPLC法。方法:色谱柱:HiQ sil-C18柱(250 mm×4.6 mm,5μm),流动相:枸橼酸(0.05 mol·L-1;三乙胺调pH 3.5～3.6)-乙腈(80:20),检测波长:293 n/n,流速:1.0 ml·min-1;柱温:30℃。结果:氧氟沙星在12.13～60.63μg·ml-1范围内线性关系良好(r=0.999 9,n=5),平均加样回收率为99.59%(n=5),RSD为0.86%。结论:此方法简便、灵敏、结果准确,可用于氧氟沙星滴耳液含量测定。     

RP-HPLC法测定通便胶囊中二苯乙烯苷的含量

目的:建立测定通便胶囊中二苯乙烯苷含量的反相高效液相色谱法.方法:采用ZORBAX ODS C18色谱柱(250 mm×4.6 mm,5μm),流动相:乙腈-水(25:75);流速:1.0 ml·min-1;检测波长:320nm;柱温:30℃.结果:二苯乙烯苷在1～2501.μg·ml-1线性关系良好(r=0.999 9);平均回收率为98.9%,RSD1.7%(n=6).结论:该方法操作简便、快速,适用于通便胶囊中二苯乙烯苷的含量测定.     

RP-HPLC测定洛伐他汀及胶囊的含量

目的 采用HPLC测定洛伐他汀及其胶囊的含量.方法 色谱柱为Agela C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.01%磷酸(60:40),流速1.0 ml·min-1.检测波长238 nm.结果 洛伐他汀的线性方程为:A=5.980×104+2.910×104C(r=0.9999),线性范围4.88～305.00 μg·ml-1,胶囊平均回收率为100.20%,RSD=0.24%(n=9).结论 所建方法准确、重复性好、操作简单,可有效地控制药品质量.     

HPLC测定复方苦参凝胶剂中苦参碱与辣椒碱的含量

目的:应用高效液相色谱法测定复方苦参凝胶剂中辣椒碱与苦参碱的含量.方法:采用WatersμBONDAPAK C18柱(3.9 mm×300mm,5 μm),乙腈-0.05 mol·L-1磷酸二氢钠溶液-三乙胺(50:50:0.05);用磷酸调整pH值至2.2为流动相;检测波长为227 nm;流速:1.0 ml·min-.结果:辣椒碱线性范围为6.25～200μg·ml-1(r=0.999 9,n=5);苦参碱线性范围为80.0～800.0 μg·ml-1(r=0.999 7,n=5).辣椒碱平均回收率为101.8%(n=9),RSD=1.8%;苦参碱平均回收率为100.7%(n=9),RSD=0.9%.结论:本方法用于凝胶剂中辣椒碱与苦参碱含量的测定简便、快速、灵敏、结果准确.     

RP-HPLC法测定复方氧氟沙星鱼肝油乳剂中氧氟沙星和甲硝唑的含量

目的:建立反相高效液相色谱法测定复方氧氟沙星鱼肝油乳剂中甲硝唑和氧氟沙星的含量.方法:采用反相高效液相色谱法,色谱柱为Diamonsii C18柱(250mm×4.6mm,5μm), 流动相为甲醇-1%醋酸铵(40∶60),流速1.0mL·min-1, 检测波长293nm.结果:甲硝唑在3.0～30.0μg·mL-1范围内线性关系良好,回归方程:Y=0.123 30 1.833 75X,r=0.999 9(n=5),平均回收率100.33%,RSD=1.49%(n=9);氧氟沙星在2.0～20.0μg·mL-1范围内线性关系良好,回归方程:Y=0.157 53 0.623 53X,r=0.999 9(n=5),平均回收率100.31%,RSD=1.19%(n=9).结论:该方法灵敏度高;专属性好;操作简便;重现性好.     

高效液相色谱法测定肤痒颗粒中红花黄色素A的含量

目的:建立肤痒颗粒中红花黄色素A含量测定的高效液相色谱法.方法:采用wfliers C<,18>色谱柱(200 mm×4.6mm,5μm),以甲醇-乙腈-0.05%磷酸溶液(20:2:78)为流动相,流速为1.0mL·mjn-1.用二极管阵列检测器检测,检测波长403 nm,柱温36℃.结果:方法的线性范围为3.698～36.98 mg·L-1(r=0.999 6),精密度RSD为0.38%(n=7),重复性RSD为0.67%(n=7),红花黄色素A的平均回收率为99.57%,RSD为0.91%(n=9).结论:本方法操作简便,结果准确、可靠,可用于肤痒颗粒中红花黄色素A的含量测定.     

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.     

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.     

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.