HPLC法同时测定口腔溃疡糊剂中盐酸丁卡因和乳酸依沙吖啶的含量

目的建立口腔溃疡糊剂中盐酸丁卡因和乳酸依沙吖啶的含量测定方法。方法采用高效液相色谱(HPLC)法,色谱柱为Thermo Hypersil GOLD C 18(250mm×4.6mm,5μm),流动相为乙腈-50mmol·L^-1磷酸二氢钾(0.5%三乙胺,磷酸调节pH 3.0),流速为1.0mL·min^-1,检测波长270nm。结果盐酸丁卡因和乳酸依沙吖啶分别在4.02~20.08μg·mL^-1和2.00~10.00μg·mL^-1范围内线性关系良好(r>0.9999),平均加样回收率分别为99.65%、100.32%,相对标准偏差(RSD)分别为0.57%、0.73%。结论该方法操作简便、结果准确、重现性好,可作为控制口腔溃疡糊剂质量的方法。     

RP-HPLC法测定口腔溃疡糊剂中盐酸丁卡因的含量

目的建立RP-HPLC法测定口腔溃疡糊剂中盐酸丁卡因含量.方法色谱柱为Shim-pack CLC-C8柱,柱温30℃;流动相为甲醇-无水乙醇-水-三乙胺(70:15:15:0.05);检测波长为310 m.结果盐酸丁卡因在20～100μg·mL-1内线性关系良好,r=0.999 7,RSD为0.98%,平均回收率为100.09%.结论方法简便、快速、准确,适用于口腔溃疡糊剂的质量控制.     

高效液相色谱法测定盐酸平阳霉素软膏的血药浓度

目的:建立人血浆中盐酸平阳霉素的HPLC测定方法,从而研究患者使用盐酸平阳霉素软膏后的透皮吸收程度.方法:500μL人血浆用150μL 10%的高氯酸沉淀后高速离心,取上清液进样20μL进行分析.流动相为甲醇-乙腈-0.002 mol·L-1戊烷磺酸钠(15:10:75),用1 mol·L-1硫酸调pH 3.5;色谱柱:ODS-C18(150 mm×4.6 mm,5μm);检测波长:254 nm;流速:1.0 mL·min-1.10名志愿受试的寻常性银屑病患者使用盐酸平阳霉素软膏后,用HPLC法测定血浆中药物浓度.结果:本实验建立的血浆中盐酸平阳霉素HPLC测定方法,血浆中杂质不干扰样品的测定,药物在0.20～0.5 mg·L-1的范围内线性关系好;最低检测为0.20 mg·L-1;回收率高于80%;高、中浓度的日间和日内变异系数均小于10.0%;低浓度的日间和日内变异系数均小于15.0%,符合生物样品分析要求.10名患者用药后血浆中盐酸平阳霉素的药物浓度均低于最低检测浓度.结论:受试者对盐酸平阳霉素的吸收在0.20 mg·L-1以下,发生药物不良反应的可能性较小,本研究中10名志愿受试者亦未出现不良反应.     

高效液相色谱法测定盐酸奈福泮片的含量

目的:建立盐酸奈福泮片中盐酸奈福泮含量的HPLC测定方法.方法:采用Dikma C18柱(150mm×4.6mm,5μm),以0.01mol·L-1庚烷磺酸钠溶液(稀磷酸调节pH为3.0)-乙腈(67:33)为流动相,流速:1.0ml·min-1;检测波长215nm;柱温:40℃.结果:线性范围为5～35μg·ml-1(r=0.999 8);平均回收率为98.9%,RSD为0.7%(n=6).结论:方法操作简便,快速准确.     

HPLC测定盐酸安非他酮片的含量

目的 采用HPLC法测定盐酸安非他酮片的含量.方法 色谱柱为迪马C18柱(250mm×4.6 mm,5μm),流动相为磷酸盐缓冲液(含0.007 mol·L-1庚烷磺酸钠、0.01 mol·L-1三乙胺、0.05 mol·L-1磷酸二氢钾)-乙腈(60:40,磷酸调pH3.2),检测波长为251 nm.结果 盐酸安非他酮在0.8～4.0 μg与峰面积呈良好的线性关系(r=0.9992),平均回收率为99.6%,RSD=0.17%.结论 所建方法准确可靠,专属性强,可为修订该制剂的质量标准提供参考.     

速效止泻胶囊定性定量检测方法研究

目的:建立速效止泻胶囊的定性定量检测方法。方法:采用TLC法鉴别速效止泻胶囊中盐酸小檗碱和拳参;采用HPLC法测定处方中盐酸小檗碱含量及拳参中绿原酸含量。盐酸小檗碱色谱条件:依利特Hypersil ODS2(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.05 mol·L-1磷酸二氢钾溶液-三乙胺(40∶60∶0.1)为流动相,流速1 mL·min-1,紫外检测波长346 nm,柱温为30℃;绿原酸色谱条件:依利特Hypersil ODS2(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.01 mol·L-1磷酸二氢钾溶液-三乙胺-磷酸(7∶93∶0.4∶0.3)为流动相,流速1 mL·min-1,紫外检测波长327 nm,柱温为30℃。结果:盐酸小檗碱和拳参薄层色谱定性鉴别特征明显;盐酸小檗碱与绿原酸含量测定,分别在2.0～6.0μg(r=0.9992)和0.1～1.8μg(r=0.9999)线性关系良好;平均回收率(n=6)分别为99.2%和102.3%,RSD分别为0.77%和1.3%。结论:本法可准确地定性、定量,有效地控制速效止泻胶囊的质量。     

高效液相色谱法测定情安喘定片中盐酸克仑特罗的含量

目的 建立高效液相色谱法测定情安喘定片中盐酸克仑特罗的含量.方法 色谱柱:Grace Smart C18(4.6mm×25mm,5μm);流动相:0.02mol·L-1磷酸二氩钾溶液-乙腈(80:20);流速:1.0mL·min-1;检测波长:243μm.结果 盐酸克仑特罗在0.015μg～0.180μg范围内线性良好,相关系数r=0.99996,平均回收率为97.4%,RSD为0.54%.结论 本法简便,准确性、重复性好,适用于盐酸克仑特罗的含量测定.     

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.     

高效液相色谱法测定复方薄荷醑中盐酸林可霉素和马来酸氯苯那敏的含量

目的:建立用HPLC法测定复方薄荷醑中盐酸林可霉素和马来酸氯苯那敏的含量。方法:采用Hypersil C18(250mm×4.6mm,5μm)色谱柱;以甲醇-0.05mol·L-1硼砂溶液-三乙胺(50∶50∶0.3,用磷酸调pH至4.2)作为流动相;流速0.8mL·min-1;柱温为35℃;检测波长为214nm。结果:盐酸林可霉素和马来酸氯苯那敏的线性范围分别为80~800mg·L-1和4~40mg·L-1(r均为0.9999),平均回收率分别为99.64%和99.39%,RSD分别为0.37%和0.53%。结论:本法操作简便,结果准确,可用于该制剂的质量控制。     

高效液相色谱法测定盐酸尼非卡兰原料及粉针的有关物质

目的:建立高效液相色谱法测定盐酸尼非卡兰原料药和冻干粉针中的有关物质.方法:采用Luna C18色谱柱(250mm×4.6mm,5μm,Phenomenex),以乙腈-0.02mol·L-1磷酸盐缓冲液(35∶65)为流动相(0.1mol·L-1氢氧化钠溶液调节pH为6.0);流速:1.2mL·min-1;检测波长:270nm;温度:室温.结果:最低检测限0.24ng,精密度(RSD)良好,日内精密度0.62%,日间精密度1.11%.结论:采用高效液相色谱法测定盐酸尼非卡兰原料药和冻干粉针中的有关物质方法简便,结果准确.     

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.     

Pharmacological treatment of COVID-19: an opinion paper

The precocity and efficacy of the vaccines developed so far against COVID-19 has been the most significant and saving advance against the pandemic. The development of vaccines has not prevented, during the whole period of the pandemic, the constant search for therapeutic medicines, both among existing drugs with different indications and in the development of new drugs. The Scientific Committee of the COVID-19 of the Illustrious College of Physicians of Madrid wanted to offer an early, simplified and critical approach to these new drugs, to new developments in immunotherapy and to what has been learned from the immune response modulators already known and which have proven effective against the virus, in order to help understand the current situation.     

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.