盐酸莫西沙星栓的制备及质量控制

目的:制备盐酸莫西沙星栓,建立质量控制方法。方法:筛选基质,采用高效液相色谱法测定盐酸莫西沙星含量,并考察其稳定性。结果:盐酸莫西沙星线性范围为0.4~3μg(r=0.9999),平均回收率为98.60%,RSD=0.61%(n=3)。结论:该处方设计合理,质量控制方法准确可靠,制剂稳定性好。     

氢溴酸加兰他敏含量测定的方法比较

目的 对氢溴酸加兰他敏不同含量测定方法进行比较研究,为完善其质量标准提供依据。方法 参照《中国药典》2020年版、《英国药典》2023年版、《欧洲药典》11.0版、《美国药典》2023年版和相关文献分别采用非水溶液滴定法、酸碱电位滴定法和高效液相色谱法测定氢溴酸加兰他敏的含量。结果 非水溶液滴定法的平均回收率为99.79%(RSD=0.46%);酸碱电位滴定法的平均回收率为100.67%(RSD=0.32%);高效液相色谱法的平均回收率分别为99.78%(RSD=0.82%)和99.85%(RSD=0.66%)。结论 酸碱电位滴定法的含量测定结果偏高,非水溶液滴定法和高效液相色谱法的测定结果较为准确,更适用于氢溴酸加兰他敏的含量测定。     

高效液相色谱法和非水电位滴定法测定注射用盐酸赖氨酸含量的比较

目的 分别建立高效液相色谱法和非水电位滴定法,用于测定注射用盐酸赖氨酸含量.方法 高效液相色谱法采用色谱柱为Phenomenex C18柱(250mm×4.6mm,5μm),流动相为甲醇-0.05 mol/L醋酸钠和醋酸溶液(60:40),流速1.0mL/min,检测波长为360nm,柱温为40 ℃;非水电位滴定法以醋酸汞和冰醋酸为溶剂,用0.1 mol/L高氯酸溶液进行滴定.结果 采用高效液相色谱法时,盐酸赖氨酸质量浓度在2.0～10.0μg/mL范围内与峰面积线性关系良好,r=0.999 5,方法精密度RSD为0.41%(n=6),平均回收率为98.8%,RSD为0.62%(n=9);采用非水电位滴定法时,方法精密度RSD为0.33%(n=6),平均回收率为99.6%,RSD为0.37%(n=9).结论 所采用的两种方法的测定结果无显著差异.高效液相色谱法分离能力高,专属性强,消耗样品量少,但该柱前衍生化高效液相色谱法操作繁杂,衍生化反应所需试剂难得;非水电位滴定法测定其电位突跃明显、易辨,操作简单、快速,测定结果精密,准确度高,成本低,能够满足其质量控制,更适合于常规检测,故采用非水电位滴定法测定该品含量,并订入其质量标准中.     

乙酰半胱氨酸胶囊的制备及质量控制

目的:制备乙酰半胱氨酸胶囊,并进行其质量控制标准的初步研究.方法:制备乙酰半胱氨酸胶囊,测定溶出度,以氧化还原滴定法及高效液相色谱法测定含量,并建立其质量控制标准.结果:乙酰半胱氨酸溶出度限度为80%;以氧化还原滴定法进行含量测定,平均回收率为99.2%,RSD为1.4%;以高效液相色谱法进行含量测定,平均回收率为99.3%,RSD为0.6%.结论:该制剂制备工艺可行,质量可控.     

HPLC法测定复方止咳糖浆中盐酸异丙嗪和氢溴酸右美沙芬的含量

目的:建立高效液相色谱法,测定复方止咳糖浆中盐酸异丙嗪和氢溴酸右美沙芬的含量.方法:采用C18柱,以0.5%三乙胺溶液(用磷酸调节pH值至3.5)-乙腈(75:25)为流动相,检测波长为278nm.结果:线性范围为盐酸异丙嗪0.1738-0.8690μg(r=0.9999);氢溴酸右美沙芬0.447-2.235μg(r=1.0000),平均回收率为盐酸异丙嗪;100.0%(RSD%=0.87%,n=9);氢溴酸右美沙芬99.8%(RSD=0.3%,n=9).结论:本方法简便,快速,专属性强,可有效的控制复方止咳糖浆中盐酸异丙嗪和氢溴酸右美沙芬的含量.     

盐酸利多卡因乳剂的制备与质量控制

目的制备盐酸利多卡因乳剂并建立其质量控制方法。方法取盐酸利多卡因及其它辅料制成乳剂,并采用高效液相色谱法测定主药含量。结果所制乳剂为乳白色半透明粘稠液体,所建立的方法能很好分离被测组分与杂质,盐酸利多卡因检测浓度在0.05~0.6mg/ml范围内线性关系良好(r=0.9998),平均回收率为99.8%,RSD=0.057%。结论本制剂制备方法简便,含量测定方法准确、可靠、灵敏,可用于其质量控制。     

复方止血栓中盐酸小檗碱的含量测定

目的建立高效液相色谱法测定复方止血栓中盐酸小檗碱含量的方法.方法甲醇-盐酸(1001)为提取溶剂,Exlipse XDB-C18色谱柱,甲醇-磷酸缓冲盐(6040)为流动相,流速为1.0 mL·min-1,柱温为35℃,检测波长为263nm.结果选用甲醇-盐酸(1001)为提取溶剂,能准确测定盐酸小檗碱的含量.盐酸小檗碱在5.0～100.0 mg·L-1范围内线性关系良好(r=0.999 8),平均回收率为97.6%,RSD为0.72%.结论该方法简便,灵敏,准确,重复性好,可用于复方止血栓的质量控制.     

RP-HPLC法测定接骨木中盐酸小檗碱的含量研究

目的采用反相高效液相色谱法建立接骨木中盐酸小檗碱含量的测定方法。方法采用反相高效液相色谱法,色谱柱:Hypersil ODS C18(4.6 mm×250 mm,5μm);流动相:甲醇-水-磷酸(25∶75∶0.2);柱温:30℃;检测波长:340 nm。结果盐酸小檗碱在4.90⁴9.0μg·mL-1范围内线性关系良好(r=0.999 8),精密度试验的RSD=0.36%,样品稳定性试验的RSD=1.08%,样品重复性试验的RSD=0.92%,平均回收率为98.68%(RSD=0.55%)。结论反相高效液相色谱法测定接骨木中盐酸小檗碱含量的方法简单、准确度高、重现性好,为制定接骨木的质量控制标准提供参考依据。     

复方护肺颗粒的制备及质量控制

目的:制备复方护肺颗粒,并建立检测方法以控制其质量。方法:采用薄层色谱法进行定性鉴别,并采用高效液相色谱法测定了岩白菜素的含量。结果:岩白菜素的含量测定的平均回收率为98.33%(RSD=2.68%)。结论:定性方法简便,定量方法准确可靠,可有效控制该制剂质量。     

高效液相色谱法测定盐酸环丙沙星栓的含量

目的:用高效液相色谱法测定盐酸环丙沙星栓的含量.方法:以 C18柱为色谱柱,0.05 mol/L枸橼酸溶液-乙腈(82 ∶18)为流动相(用三乙胺调节 pH值至3.5),检测波长为277 nm.结果:线性范围为 0.004～ 0.032 mg/mL,r=0.999 7(n=5),平均回收率为 99.93%,RSD=0.39%.结论:高效液相色谱法简便、准确,适用于盐酸环丙沙星栓的质量控制.     

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.     

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.