氧氟沙星胶囊含量测定HPLC法的改进

目的　采用HPLC法改进的流动相系统测定氧氟沙星胶囊中氧氟沙星的含量。方法　色谱柱 :TechsphereC1 8ODS柱(1 5 0mm× 4 6mm ,5 μm) ,流动相 :0 0 5mol·L-1 枸橼酸 -乙腈 -四乙胺 (70∶2 8∶2 ) ,流速 :0 8ml·min-1 ,UV检测波长 :2 93nm。结果　氧氟沙星在 2 0 4～ 1 0 2 0mg·L-1 范围内 ,浓度与峰面积线性关系良好 (r =0 9999) ,日内RSD =1 0 7% (n =5 ) ,日间RSD =1 2 3% (n =3)。平均回收率为 99 98% (n =5 )。结论　改进后方法简便、快速、结果准确 ,可用于氧氟沙星胶囊的质量控制     

RP-HPLC法测定乳酸左氧氟沙星氯化钠注射液中主药含量及有关物质

目的: 建立乳酸左氧氟沙星氯化钠注射液中主药及有关物质的含量测定方法.方法: 采用高效液相色谱法,以Lichrospher-C18柱(200 mm×4.6 mm,5 μm)为色谱柱;乙腈:1 mol·L-1醋酸铵-0.05 mol·L-1枸橼酸缓冲液(1: 79,用三乙胺调pH值为4.00)(20: 80)为流动相;流速为1.0 ml·min-1;UV检测波长为293 nm,乳酸左氧氟沙星含量测定采用外标法,有关物质检查采用归一化法.结果: 建立的色谱方法使有关物质与主药分离良好,乳酸左氧氟沙星浓度在5.0～50.0 μg·mL-1内线性关系良好,平均回收率为99.90%,RSD为0.28%.结论: 此法专属性强,操作方便,结果准确,重现性好,可用于乳酸左氧氟沙星氯化钠注射液中主药的含量测定及有关物质的检查.     

HPLC法检查氧氟沙星葡萄糖注射液中5-HMF的研究

目的 研究氧氟沙星葡萄糖注射液中5-HMF的检查方法.方法 采用HPLC法,色谱柱:SHIMADZU ODS(150 mm×4.6 mm,5μm);流动相:0.05 mol/L枸橼酸溶液(用三乙胺调pH值至4.0)-乙腈(79∶21);检测波长:284 nm;柱温:30℃.结果 可分离5-HMF,分离度为:3.0.结论 本法简便,灵敏,准确,排除了氧氟沙星等成分的干扰,可用于氧氟沙星葡萄糖注射液中5-HMF的检查和质量控制.     

高效液相色谱法测定左氧氟沙星滴鼻液中左氧氟沙星的含量

目的 建立高效液相色谱法测定左氧氟沙星滴鼻液中左氧氟沙星的含量.方法 采用美国Waters高效液相色谱仪,流动相为枸橼酸(0.05 mol·L-1枸橼酸溶液用三乙胺调节Ph值至4.0)-乙腈(79∶ 21),流速1.0 ml·min-1,检测波长293 nm.结果 左氧氟沙星在50～500 mg·L-1范围内,线性关系良好,r=0.9995.回收率为99.2%.结论 本法可准确测定左氧氟沙星滴鼻液中左氧氟沙星的含量,适用于产品的质量控制.     

HPLC法测定盐酸多西环素缓释药线中盐酸多西环素的含量

目的 建立盐酸多西环素缓释药线中盐酸多西环素的含量测定方法.方法 采用HPLC法测定药线中盐酸多西环素的含量.Alltima C18(4.6 mm×250 mm, 5 μm)柱,流动相为0.05 mol·L-1草酸铵溶液∶N,N-二甲基甲酰胺∶0.2 mol·L-1磷酸氢二铵溶液(65∶30∶5),用氨试液调节pH值为8.0±0.2,检测波长280 nm,流速为1.0 ml·min-1.结果 盐酸多西环素在49～490 mg·L-1范围内线性关系良好,r=0.9997,A=43767C 562001;平均回收率为98.72%,RSD＝1.31%(n=6 ).结论 该法简单可行,结果准确,可用于该制剂的质量标准检测.     

高效液相法测定吡拉西坦葡萄糖注射液的含量

目的探讨吡拉西坦葡萄糖注射液的含量测定方法.方法用HPLC法测定吡拉西坦葡萄糖注射液中吡拉西坦的含量.Waters公司色谱柱:SymmetryShieldTM RP18,5 μm,250mm×4.6 mm;柱温25℃,检测波长:220 nm,流动相:水,流速:1 L·min-1,进样量:20μl.结果标准曲线在10～50 mg·L-1范围内有良好线形关系(r=0.999 6),最低检测浓度为20μg·L-1,平均回收率为99%～100%之间,日内日间RSD均小于0.6%.结论该方法简便,快速准确.     

左氧氟沙星注射液的制备及质量控制

目的:制备合格的盐酸左氧氟沙星氯化钠注射液.方法:用氯化钠调节注射液渗透压,用盐酸调节pH值,使pH值在4.0～6.0范围内;采用紫外分光光度法测定左氧氟沙星的含量.结果:制备的左氧氟沙星注射液符合国家标准,其回收率为99.36%,RSD=0.945%(n=5).结论:制备方法合理,左氧氟沙星注射液质量可控,稳定性好.     

5%葡萄糖注射液中外源性抗氧剂的测定

目的建立HPLC法测定聚丙烯瓶装5%葡萄糖注射液中抗氧剂1010和168的含量,研究抗氧剂向注射液迁移情况。方法采用伊利特C18柱（250 mm×4.6 mm,5μm）为色谱柱;乙腈-四氢呋喃-水（62∶30∶8）为流动相;流速：1.5 ml·min-1;检测波长：276 nm。结果抗氧剂1010在0.61～363.66 mg·L-1范围内线性关系良好,平均回收率为91.07%,RSD=1.48%;抗氧剂168在1.21～362.66 mg·L-1范围内线性关系良好,平均回收率为93.53%,RSD=1.07%。结论聚丙烯瓶材料中抗氧剂向5%葡萄糖注射液中进行了迁移,有定量控制的必要,本法快速、准确,可用于测定抗氧剂1010和168的含量。     

0.9%氯化钠注射液中两种酯类阻氧剂的测定

目的用高效液相色谱法测定聚丙烯包装的0.9%氯化钠注射液中两种酯类阻氧剂(1010和168)的含量,研究工业阻氧剂向制剂中浸出情况。方法采用C18柱(250 mm×4.6 mm)为色谱柱;乙腈-乙醇-四氢呋喃(61∶10∶29)为流动相;流速:1.5 ml·min-1;紫外检测器检测波长:275 nm;结果阻氧剂1010在0.6～240 mg·L-1范围内线性关系良好,平均回收率为88.43%,RSD=3.90%;阻氧剂168在1.2～240 mg·L-1范围内线性关系良好,平均回收率为91.27%,RSD=3.57%。结论在0.9%氯化钠注射液中存在包装材料中的阻氧剂,需要加强控制,该法简便、有效,可以用来对阻氧剂定量。     

HPLC测定氧氟沙星麻黄碱滴鼻液的含量

目的建立测定氧氟沙星麻黄碱滴鼻液含量的方法。方法采用HPLC法同时测定滴鼻液中氧氟沙星与麻黄碱的含量。色谱柱为AlltimaC18(250mm×4.6mm,5μm);柱温35℃;流动相为0.05mol.L-1醋酸铵溶液(用三乙胺调节pH4.0)-乙腈(85∶15);流速1.0ml.min-1;检测波长254nm;检测灵敏度为0.1AUFS,进样量20μl。结果氧氟沙量在1.5μg.ml-1~0.75mg.ml-1浓度范围内,峰面积与浓度的线性关系良好(r=0.9999),平均回收率为101.2%;麻黄碱在5μg.ml-1~2.5mg.ml-1范围内,峰面积与浓度的线性关系良好(r=0.9999),平均回收率为101.4%;重复性试验的RSD=0.5%(n=9)。结论所用方法快速、简便,精密度好,灵敏度高,可作为氧氟沙星麻黄碱滴鼻液的含量控制方法。     

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.     

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.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

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.