HPLC法测定甲磺酸帕珠沙星原料及其制剂含量

目的:采用高效液相色谱法测定甲磺酸帕珠沙星原料及其制剂含量.方法:Hypersil C18(5 μm,4.6 mm×250 mm)色谱柱,0.1%磷酸溶液(加磷酸氢二钾80.5 mg)-乙腈(85:15)为流动相,流速1.0ml·min-1,柱温30℃,检测波长243 nm.结果:甲磺酸帕珠沙星在5～500μg·ml-1内与峰面积呈良好的线性关系.甲磺酸帕珠沙星原料(3批)加样回收率99.2%甲磺酸帕珠沙星注射液加样回收率均值为100.1%;甲磺酸帕珠沙星氯化钠注射液加样回收率均值为99.7%.结论:采用HPLC测定原料及其制剂中甲磺酸帕珠沙星含量方法简便,结果可靠.     

复方甲磺酸帕珠沙星滴眼液的制备及质量控制

目的制备复方甲磺酸帕珠沙星滴眼液,并建立质量控制方法。方法以甲磺酸帕珠沙星、氯化钠、地塞米松磷酸钠、羟苯乙酯制备复方甲磺酸帕珠沙星滴眼液;采用高效液相色谱法测定其中甲磺酸帕珠沙星的含量。结果甲磺酸帕珠沙星检测浓度在20.0～80.0μg/ml范围内线性关系良好（r=0.9999）,平均回收率为97.7%（RSD=1.96%,n=6）。结论本方法简便？准确？重现性好,可用于甲磺酸帕珠沙星滴眼液的质量控制。     

双波长法测定凝胶剂中甲磺酸帕珠沙星的含量

目的：建立甲磺酸帕珠沙星凝胶中甲磺酸帕珠沙星含量的测定方法。方法：采用双波长紫外分光光度法,测定波长为247nm,参比波长为232nm,测得吸收度差值（ΔA）为定量依据。结果：甲磺酸帕珠沙星在3～10μg/ml浓度范围内线性良好,相关系数为0.9993,平均加样回收率为100.3%,RSD为1.4%（n=9）。结论：本方法测定甲磺酸帕珠沙星凝胶的含量,可消除辅料的干扰,其方法简便、快速、准确。     

甲磺酸帕珠沙星注射液治疗泌尿系统感染的疗效评价

目的分析和评价甲磺酸帕珠沙星注射液治疗泌尿系统感染的疗效及其安全性。方法选取50例泌尿系统诊断明确的患者,随机分成甲磺酸帕珠沙星组与左氧氟沙星组,分别以甲磺酸帕珠沙星注射液和左氧氟沙星作为对照治疗,治疗7～14d,观察其疗效及安全性。结果甲磺酸帕珠沙星组与左氧氟沙星组的痊愈率分别为72%和64%,显效率分别为28%和36%,甲磺酸帕珠沙星疗效有略升高优势,但没有统计学上的差异(P>0.05),表明两者在治疗泌尿系统的感染时具有相当的药理效能,其总有效率均为100%。结论甲磺酸帕珠沙星注射液的临床疗效确切,安全性高,适应于中、重度泌尿路感染,在临床值得推广和使用。     

司帕沙星中8种有机溶剂残留量的测定

目的建立测定司帕沙星中8种有机溶剂残留量的方法。方法采用静态顶空气相色谱-质谱法,程序升温,初始温度40℃维持5 min,以30℃.min-1升温至200℃,保持3 min,溶剂为二甲亚砜,色谱柱为HP-INNOWAX毛细管柱(30 mm×0.25 mm,0.25μm),载气为氮气,测定司帕沙星中甲醇、二氯甲烷、乙腈、三氯甲烷、甲苯、吡啶、二甲苯和N,N-二甲基甲酰胺8种有机溶剂残留量。结果在确定的色谱条件下各组分能基线分离,线性关系良好,平均回收率为94.1%～101.1%。最低检测限为0.003～0.230μg.mL-1。结论该方法灵敏度和准确度均达到有机溶剂残留量检测的要求,可用于司帕沙星中8种有机溶剂残留量的测定。     

甲磺酸帕珠沙星原料药的急性毒性作用研究

目的 研究甲磺酸帕珠沙星原料药的急性毒性作用,指导临床安全用药.方法 按照〈化学药物急性毒性试验技术指导原则〉中方法进行试验.结果 甲磺酸帕珠沙星原料药小鼠一次性灌胃最小致死量（MLD）大于5000mg/kg,小鼠静脉注射半数致死量（LD50）为439.35mg/kg,95%可信限为399.99～482.58 mg/kg.结论 甲磺酸帕珠沙星毒性小,使用安全范围大.     

毛细管气相色谱法测定甲磺酸帕珠沙星中有机溶剂残留量

目的建立测定甲磺酸帕珠沙星中甲醇、氯仿、二氧六环和N,N-二甲基甲酰胺残留量的气相色谱方法。方法采用SPB-5石英毛细管柱为色谱柱;以水为溶剂,正丙醇为内标;柱温为90℃;进样口温度为220℃;FID检测器温度为250℃;载气为氮气;柱流量为1mL.min-1;分流比为30:1;进样量为1μL。结果甲醇、氯仿、二氧六环和N,N-二甲基甲酰胺分别在0.025～0.15,0.0015～0.009,0.0095～0.057,0.022～0.132mg.mL-1的浓度内线性关系良好(r>0.999);加样回收率分别为99.5%,100.4%,99.3%,101.2%;检测限分别为1,1.2,1,1.8ng。结论该方法简便、快速、准确,适用于本品有机溶剂残留量的测定。     

甲磺酸帕珠沙星凝胶的制备及含量测定

目的:制备甲磺酸帕珠沙星凝胶并建立其含量测定方法.方法:以卡波姆-940为基质制备凝胶,用紫外分光光度法在λ=247 mm处测定甲磺酸帕珠沙星凝胶的含量.结果:甲磺酸帕珠沙星的pH值6.0～7.0,线性范围为2.0～16.0 μg·mL-1,平均回收率99.75%,RSD为0.41%.其它试验均符合凝胶剂的有关规定.结论:本制剂工艺简单,质量可控,性质稳定,有良好的临床使用价值.     

注射用甲磺酸帕珠沙星在常用输液中的稳定性考察

目的考察甲磺酸帕珠沙星粉针剂在常用输液中的稳定性,并预测其室温贮存有效期。方法采用高效液相色谱法测定甲磺酸帕珠沙星含量,用初匀速法预测其有效期。结果甲磺酸帕珠沙星粉针剂在生理盐水或葡萄糖注射液中12 h内稳定,但不宜长时间放置。初匀速法实验结果预测甲磺酸帕珠沙星葡萄糖注射液有效期为30 h,甲磺酸帕珠沙星生理盐水注射液有效期为12 h。结论初匀速法预测甲磺酸帕珠沙星有效期简便、迅速。用初匀速法预测甲磺酸帕珠沙星稳定性及其有效期为临床用药提供了依据。     

甲磺酸帕珠沙星壳聚糖滴鼻剂的制备与质量控制

目的研究甲磺酸帕珠沙星壳聚糖滴鼻剂的制备方法并建立其质量控制方法。方法以壳聚糖为增稠剂和增效剂、甲磺酸帕珠沙星为主药制备滴鼻剂,采用高效液相色谱法测定主药含量,并对其稳定性进行考察。结果该产品的处方和制备工艺简单,质量稳定,甲磺酸帕珠沙星质量浓度在20.0～80.0μg/mL范围内与峰面积线性关系良好,r=0.9999(n=6);平均回收率为98.62%,RSD为0.53%(n=9)。结论滴鼻剂可作为甲磺酸帕珠沙星制剂新品种的开发研究对象。     

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.