高效液相色谱法同时测定氨酚曲马多片中2种组分的含量

目的:建立高效液相色谱法测定氨酚曲马多片中盐酸曲马多和对乙酰氯基酚的含量。方法:以DiamonsilTMC18柱为色谱柱;采用甲醇-0．02 mol·L-1磷酸二氢钾溶液(45:55)为流动相,流速1．0 mL·min-1,检测波长为220 nm。结果:本方法可同时测定2个组分含量。盐酸曲马多和对乙酰氨基酚分别在10．8～37．8μg·mL-1和91．0～318．5μg·mL-1浓度范围内,峰面积与其浓度呈良好的线性关系,平均回收率和RSD范围分别为100．2％～100．5％和0．33％～0．46％;99．7％～100．4％和0．39％～0．54％。结论:本法简便、快速、结果准确,适用于该复方制剂的含量测定。     

白细胞介素-2前体脂质体的初步研究

目的:制备白细胞介素-2(IL-2)前体脂质体并考察其稳定性。方法:采用冷冻真空干燥法制备IL-2前体脂质体,采用Sephadex~(TM) G-50柱分离脂质体,MTT比色法测定活性,激光粒度仪测定粒径。结果:制备的IL-2前体脂质体为白色的非定型粉末,粒径分布在0．1～1．0μm,包封率为95．5%,活性5．0×10~6IU·g~(-1)。结论:本方法制备的前体脂质体制剂有较高的包封率,贮存稳定,粒度分布良好。     

氢地油乳剂的制备及质量控制

目的:制备氢地油乳剂并建立其质量控制方法。方法:采用乳化法,以盐酸丁卡因为主药制备氢地油乳剂;采用紫外分光光度法测定其中盐酸丁卡因的含量;考察3批样品的稳定性。结果:所制制剂为白色乳状物;盐酸丁卡因检测浓度的线性范围为3.168～9.504μg.mL-1(r=0.9999),平均回收率为99.68%(RSD=0.49%)。3批样品经留样试验考察,质量稳定。结论:该制剂制备方法简便,含量测定准确,质量在保质期内稳定可控。     

胰激肽原酶测定方法的改进

目的改进胰激肽原酶效价测定方法,提高检验质量与速度。方法采用酶标仪替代紫外分光光度计测定胰激肽原酶效价。结果酶标仪测定结果与紫外分光光度计一致。结论采用酶标仪测定胰激肽原酶可减少样品使用量,提高检验工作效率。     

RP-HPLC法测定盐酸拓扑替康及制剂含量和有关物质

目的:建立高效液相色谱法测定盐酸拓扑替康(TPT)及制剂中有关物质和含量。方法:采用十八烷基硅烷键合硅胶为填充剂,0．5％磷酸和0．5％正丁胺(v／v)溶液-甲醇(60:40)为流动相,流速1．0 mL·min-1,检测波长为267 nm。结果:盐酸拓扑替康与有关物质分离良好,线性范围为10-100μg·mL-1(r=0．9999),最低检出量为0．02 ng。方法精密度(RSD)为 0．41％(n=9)。制剂平均回收率为99．3％。结论:方法快速简便,准确,可用于原料及制剂中有关物质和含量的测定。     

盐酸司帕沙星原位胶化滴眼剂的制备及质量控制

目的:制备盐酸司帕沙星原位胶化滴眼剂并建立其质量控制方法。方法:以硼酸为渗透压调节剂、海藻酸钠为胶化剂制备滴眼剂;采用紫外分光光度法测定其中主药的含量,并考察其稳定性。结果:所制制剂为无色或淡黄色澄明液体,鉴别、检查均符合2005年版《中国药典》中的相关规定;盐酸司帕沙星检测浓度的线性范围为3·0～8·0μg·mL-1,平均回收率为99·82(RSD=0·236%,n=6)。本品加速、留样试验中各指标无明显变化,温度和光照对样品有轻微影响。结论:本制剂制备工艺简便可行,质量稳定可控。     

氯诺昔康凝胶的制备及质量控制

目的:制备氯诺昔康凝胶并建立其质量控制方法。方法:以壳聚糖为辅料制备凝胶;采用高效液相色谱法测定其中主药的含量,并采用加速试验、离心法考察其稳定性。结果:所制制剂涂展性好;氯诺昔康检测浓度的线性范围为12.5～125.0μg·mL-1,平均回收率为100.02%(RSD=1.18%) ;稳定性指标均符合规定。结论:本制剂制备工艺简单,质量稳定、可控。     

HPLC法测定咖普苯片中咖啡因、盐酸普萘洛尔、苯妥英钠3组分的含量

目的 :建立同时测定咖普苯片中咖啡因、盐酸普萘洛尔、苯妥英钠 3组分含量的高效液相色谱法。方法 :采用In ertsil-ODS柱 ,流动相为甲醇 -水 - 0 2mol·mL-1磷酸二氢钾溶液 (5 0∶43∶2 ) ,流速 1 0mL·min-1,检测波长 2 30nm ,外标法计算。结果 :线性范围分别是 :咖啡因 2 0～ 16 0 μg·mL-1,r =0 9998;盐酸普萘洛尔 3～ 2 4μg·mL-1,r =0 9995 ;苯妥英钠 35～ 2 80 μg·mL-1,r =0 9999。回收率 :咖啡因 10 0 3 % ;盐酸普萘洛尔 10 0 7% ;苯妥英钠98 6 %。结论 :本方法分离效果好 ,辅料无干扰 ,快速、简便 ,适用于该制剂 3组分的同时测定     

聚维酮碘新制剂的制备及质量控制

目的:制备聚维酮碘新制剂并建立其质量控制方法。方法:制备独立包装的聚维酮碘片剂及缓冲溶液,采用电位滴定法测定混合后制剂中碘的含量,同时考察其稳定性。结果:所制制剂固相为棕红色片剂,液相为pH约5.8的无色澄清溶液;混合后制剂溶液中平均有效碘含量为95.24mg;稳定性考察中,10h内有效碘含量测定结果平稳。结论:本制剂制备工艺简单可行,质量稳定可控。     

注射用替加环素的制备、质量控制及稳定性考察

目的:制备注射用替加环素,并建立其质量控制方法及考察其稳定性。方法:筛选制备条件、辅料和中间体溶液的pH值,确定注射用替加环素的制备工艺和处方组成;采用高效液相色谱法测定其含量及有关物质,并对制剂进行稳定性考察(影响因素、加速试验和长期留样试验(24个月))。结果:制备条件以2～8℃为宜,处方中选用乳糖为赋形剂,其与主药用量比为2:1,中间体溶液的pH以7·5～8·5为宜;替加环素进样量线性范围为0·103～10·30μg(r=0·9999,n=7);低、中、高浓度平均回收率为99·9%、100·2%、100·2%,RSD=1·20%、0·50%、0·72%。稳定性考察期内各指标未见明显变化。结论:该制剂处方工艺可行,质量可控,稳定性较好。     

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.     

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.     

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.