高效液相色谱法测定硫酸罗通定注射液中有关物质

目的建立硫酸罗通定注射液中有关物质的测定方法。方法以十八烷基硅烷键合硅胶为填充剂，乙腈-磷酸盐缓冲液（pH=6、8）-三乙胺（60：40：1，用30％磷酸溶液调节pH值至6．8±0．05）为流动相，检测波长为280nm，进样量为20μL。结果罗通定进样量在5～30μL范围内，质量浓度在12～36μg／μL范围内与峰面积线性关系良好，r=0．99940结论高效液相色谱法测定本品中有关物质，专属性强，灵敏度高，重现性好。     

毛细管色谱法测定洛美沙星中的有机溶剂残留量

目的：建立毛细管气相色谱法测定洛美沙星中的有机溶剂残留量。方法：用INNOWAX毛细管气相色谱柱，FID检测器，以2-戊酮为内标进行测定。结果：乙酸乙酯、四氢呋喃、乙醇、乙腈的线性范围分别为0～80μg／ml(r=0．9997)、0～11．52μg／ml(r=0．9996)、0～80μg／ml(r=0．9997)，0～6．56μg／ml(r=0．9996)；平均回收率分别为100．5％、100．1％、101．2％、100．1％；RSD分别为1．30％、0．9％、1．18％和1．23％(n=9)。结论：本方法简单、准确、灵敏度高、重现性好，适用于洛美沙星中有机溶剂残留量的测定。     

HPLC法测定罗通定及硫酸罗通定注射液中的有关物质

目的：建立HPLC法测定罗通定及硫酸罗通定注射液中的有关物质检查方法。方法：色谱柱为Agilent ZORBAX SB-C18（250mm×4．6mm，5μm）柱；流动相为：乙腈-磷酸盐缓冲液（pH6．8）-三乙胺（60：40：1）（用磷酸调pH至6．8）为流动相；检测波长：280nm；流速为：1mL·min^-1。结果：罗通定与其有关物质能够完全分离。最低检出限为1．2ng。结论：方法简便、准确，灵敏，可用于罗通定及硫酸罗通定注射液中的有关物质检查。     

复方厄贝沙坦片中厄贝沙坦和氢氯噻嗪的HPLC测定

建立同时测定复方厄贝沙坦片中厄贝沙坦和氢氯噻嗪含量的HPLC方法。用Inertsil ODS-3色谱柱，流动相为乙腈-0．08mol／L磷酸溶液(用三乙胺调至pH5．0)(40：60)，检测波长225nm。厄贝沙坦和氢氯噻嗪分别在15～135μg／ml(r=0．9999)和1．2～10．8μg／ml(r=0．9999)浓度范围内线性关系良好，方法平均回收率分别为100．0％(RSD=0．46％)和100．5％(RSD=0．49％)。     

高效液相色谱法测定消银片含量

目的：用高效液相色谱法测定消银片含量；方法：ODS柱，以乙腈：0．1％磷酸溶液(40：60)为流动相，于220nm波长处检测，流速1．0ml／min；结果：该方法在50μg／ml～460μg／ml范围内，峰面积与浓度呈良好的线性关系(r=0．9998)，重复性试验RSD=1．21％(n=6)；结论：方法简便快速、重现性好。     

HPLC法测定血浆及组织中替硝唑、环丙沙星和消炎痛的含量

目的：建立用HPLC测定血浆和组织中替硝唑、环丙沙星和消炎痛的方法，为研究外用复方制剂的药代动力学提供依据。方法：取血浆或组织匀浆200μl，加甲醇400μl沉淀蛋白，离心后取上清液450μl，于60℃通空气吹干，残渣用50μl甲醇溶解，离心后进样20μl。色谱条件：C18-ODS柱，替硝唑与消炎痛同时测定，流动相为甲醇-水(55：50)，流速0．8ml／min，检测波长310nm(0-5．4min)、277nm(5．4-10min)，环丙沙星单独测定，流动相为甲醇-水(40：60)，含0．12％NH4H2PO4，H3PO4调pH3．6 0．2)，流速0．8ml／min，检测波长277nm。结果：替硝唑浓度在0．02-4．0μg／ml范围内与峰面积线性关系良好，r=0．9998，其日内日间差异性≤6．3l，平均回收率为92．05％-93．80％；环丙沙星浓度在0．02-4．0μg／ml范围内与峰面积线性关系良好，r=0．9984，其日内日间差异性≤4．76，平均回收率在99．77-104．23间；消炎痛浓度在0．06～8．0μg／ml范围内与峰面积线性关系良好，r=0．9998，其日内日间差异性≤5．45，平均回收率为98．96％-110．00％。结论：该方法灵敏、可靠，适于测定血浆和组织中替硝唑、环丙沙星和消炎痛的含量。     

盐酸吡格列酮的HPLC测定

用HPLC测定盐酸吡格列酮及其有关物质的含量。采用C18色谱柱，以乙腈-水-醋酸(50：50：0．12，用氨试液调至pH6．0)为流动相，流速1．0ml／min，检测波长225nm。盐酸吡格列酮在1-200μg／ml范围内线性良好，平均回收率99．3％(RSD=0．09％)，日内和日间精密度(RSD)分别为0．75％和0．26％。     

HPLC法同时测定感冒喷雾剂主药含量

目的：建立同时测定感冒喷雾剂中盐酸萘甲唑林和马来酸氯苯那敏含量的HPLC法。方法：采用ODS柱，以乙腈-1．0％十二烷基硫酸钠-冰醋酸(65:35:0．3)为流动相，检测波长为264nm。结果：盐酸萘甲唑林Y=19132．4X 11486．8，r=0．9999(n=5)，线性范围15．18～25．31μg／ml，回收率99．6％,RSD0．60％(n=5)。马来酸氯苯那敏Y=14214．3X 45201．5，r=0．9999(n=5)，线性范围76．56～127．6μg／ml，回收率99．8％。RSD0．63％(n=5)。结论：本法方便、快捷、准确、精密度高，适用于感冒喷雾剂的含量测定。     

高效液相色谱法测定氯霉素滴眼液的含量

目的：采用HPLC法测定氟霉素滴眼液的含量。方法 采用CDS Dimard色谱柱，水：甲醇：氨水(58：40：2)为流动相，用gAC调节PH为6．4，紫外检测波长278nm。结果：线性范围为25μg／ml—150μg／ml，r=0．9994，平均回收率为100．4% RSD为1．0％(n=5)，符合要求。结论本法操作简便，重现性好，结果准确可靠。     

固相萃取-HPLC法快速测定苯妥英钠及卡马西平的血药浓度

目的 应用固相萃取(SPE)-反相HPLC法同时测定苯妥英钠(PHT)及卡马西平(CBZ)血药浓度。方法 将1ml血浆样品在GDX-403固相萃取柱上进行固相萃取，洗脱液混匀后直接进样。色谱条件：色谱：Hypersil BDS C18柱，流动相：甲醇：水=48：52，检测波长：235nm，流速：1ml／min，柱温：25℃，内标：非那西丁。结果 PHT在4．10-41．0μg／ml范围内线性良好(γ=0．9999)；CBZ在2．50-24．96μg／ml范围内线性良好（γ=0.9998)，方法平均回收率各为101.77％和101．87％，日内及日间误差分别小于4．13%和49.8％，最低检测浓度为：1．025μg／ml和0．156μg/ml。结论 该方法、准确、快速，可用于PHT及CBZ血浆浓度的同时测定。     

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.