高效液相色谱法测定盐酸决奈达隆片的溶出度

目的 应用高效液相色谱技术建立盐酸决奈达隆片溶出度的测定方法. 方法 采用Agilent ZORBAX Eclipse Plus C18 色谱柱(100 mm×4.6 mm,3.5 μm)进行分离,以2 mmol.L^-1磷酸二氢钠(氢氧化钠调至pH 7.0)-甲醇-乙腈(20:30:50)为流动相,流速1.5 mL.min^-1,检测波长290 nm. 溶出度采用浆法,以水900 mL为溶出介质,转速125 r.min^-1. 结果 辅料不干扰决奈达隆的测定;决奈达隆的线性相关系数(r)为1.000 0;检出限(以决奈达隆游离碱计)为0.19 mg.L^-1;精密度和12 h稳定性RSD均<1%;回收率101.2%～102.1%. 3批样品溶出度的均一性良好(RSD<7%),平均溶出度均＞75%. 结论 该方法准确、简单、快速,可作为盐酸决奈达隆片溶出度的测定方法.     

高效液相色谱法测定石杉碱甲胶囊溶出度

目的 建立石杉碱甲胶囊溶出度的高效液相色谱 方法 . 方法 以盐酸溶液（9→1 000）100 mL为溶出递质,转速为35 r&#8226;min^-1,取样时间为30 min,采用溶出度第三法测定. 结果 石杉碱甲在0.13～1.02 μg&#8226;mL^-1的浓度范围内,线性关系良好. 线性方程为：A＝103.95C-0.15 （r＝1.000 0）;平均回收率为98.0%（RSD＝0.7%）;4批样品30 min平均溶出度均＞80%. 结论 该 方法 简便、准确、重现性好,可用于石杉碱甲胶囊的质量控制.     

氢溴酸加兰他敏分散片溶出度的测定方法

目的:研究并建立氢溴酸加兰他敏分散片溶出度测定方法.方法:按中国药典2000年版附录中溶出度项下第三法,分别以水、1%盐酸、5%乙醇等3种溶出介质进行氢溴酸加兰他敏分散片的溶出试验,采用HPLC法测定溶出介质中氢溴酸加兰他敏分散片的浓度.结果:在10～100μg·ml-1范围内,线性关系良好(r=0.999 7),平均回收率为100.2±1.30,RSD为1.5%.氢溴酸加兰他敏分散片30 min的溶出量大于标示量的90%.结论:所建立的溶出度测定法简单、准确、可靠,可作为控制氢溴酸加兰他敏分散片的质量标准之一.     

4种头孢泊肟酯片的体外溶出度比较

目的考察4种市售头孢泊肟酯片的体外溶出度，评价其片剂质量。方法采用《中华人民共和国药典》(2000年版)溶出度测定法第2法，以盐酸溶液(9→1 000)为溶剂，转速分别为100和50 r·min^-1，进行溶出度测定实验。采用紫外分光光度法测定溶出量，测定波长为263 nm。计算累积溶出率。结果 线性范围为3～18 μg·mL^-1，r＝ 0.999 6。45 min内4种待测药物在盐酸溶液(9→1 000)中的累积溶出百分率均＞70.0%。转速为100 r·min^-1时，4种头孢泊肟酯片30 min溶出率均＞90.0%；转速为50 r·min^-1时，4种头孢泊肟酯片45 min内的溶出率均＞70.0%。结论4种被测头孢泊肟酯片均符合质量标准，但不同生产厂家的产品之间有差异。     

高效液相色谱法测定缬沙坦分散片的体外溶出度

目的考察缬沙坦分散片的体外溶出度。 方法采用《中华人民共和国药典》(2000年版)溶出度测定第一法，以0.05 mol·L^-1的磷酸二氢钾溶液(pH值＝6.8)为溶出介质，采用高效液相色谱法［固定相：Nucleosil C18色谱柱(4.6 mm×250 mm，5 μm)；流动相：乙腈∶水∶醋酸 (48∶52∶0.1)；流速：1.0 mL·min^-1；测定波长：270 nm；柱温：室温］测定缬沙坦分散片同一批号不同组次和不同批号的溶出度。结果缬沙坦分散片20 min内累积体外溶出率＞90%。结论缬沙坦分散片的体外溶出特性好，质量稳定。     

洛美利嗪片体外溶出度研究

目的建立洛美利嗪片体外溶出度的测定方法。方法以0.1 mol·L^-1盐酸溶液为溶出递质，采用小杯法，转速为75 r·min^-1，温度为(37.0±0.5)℃，进行累积溶出百分率测定。用紫外分光光度法在225 nm的波长处测定。结果洛美利嗪在盐酸溶液中8～20 μg·mL^-1范围内线性关系良好，平均回收率为100.4%，RSD＝0.7%(n＝5)。洛美利嗪片15 min内溶出＞90.0%，45 min时溶出度RSD＜2.0%。结论洛美利嗪片溶出速度快，溶出均一性好。     

氢溴酸高乌甲素分散片的处方优化及制备

目的:制备氢溴酸高乌甲素分散片,并对其处方进行优化。方法:湿法制粒压片法制备氢溴酸高乌甲素分散片。以崩解时限、口感、片面光洁度为指标进行处方筛选,并采用正交实验设计优化处方。结果:最佳处方为氢溴酸高乌甲素-阿司帕坦-薄荷香精5∶5∶1;交联聚维酮6%;乳糖:微晶纤维素2∶1;硬度5 kg。所制片剂片面光洁,口感良好,崩解分散快,分散均匀性符合药典相关要求,释药速度较普通片快,10 min内溶出即达80%以上。结论:优化后的氢溴酸高乌甲素分散片制备方法简单,崩解迅速,分散均匀,溶出速度快,达到了设计要求。     

复方阿莫西林胶囊的制备与质量控制

目的 制备复方阿莫西林胶囊,并探讨其质量控制方法 . 方法 以湿法制粒制备复方胶囊,采用高效液相色谱法测定复方胶囊的含量与溶出度. 结果阿莫西林与氨溴索回归方程的线性范围分别为80～320 μg.mL^-1和4.8～19.2 μg.mL^-1,加样回收率分别为96.72%和104.17%,RSD分别为1.84%和0.57%. 3批样品的含量均>90%,45 min溶出度>80%. 结论 复方阿莫西林胶囊的含量与溶出度均符合2010年版《中华人民共和国药典》要求,该检测方法 准确、简便,分离效果好,可用于该复方胶囊的质量控制.     

盐酸金刚烷胺片溶出度测定方法研究

目的 建立盐酸金刚烷胺片的溶出度测定方法。方法 釆用紫外 可见分光光度法测定盐酸金刚烷胺片的溶出度，测定波长为（412±1）nm。结果 在2.5～15.0 μg·mL^-1的浓度范围内与吸光度值呈良好的线性关系（r=0.999 5，n=6），平均回收率为99.82%，RSD=0.87%（n=6）。结论 该方法灵敏、准确可靠、重现性好，可用于盐酸金刚烷胺片的溶出度测定。     

高效液相色谱法测定罗红霉素片与罗红霉素分散片溶出度

目的建立罗红霉素片与罗红霉素分散片的溶出度测定方法。方法采用转篮法，以醋酸盐缓冲液(pH5.5)为溶出介质，转速为100 r&#8226;min 1，经45 min取样，取样后采用高效液相色谱法测定。结果罗红霉素在0.02～0.20 mg&#8226;mL 1范围内呈较好的线性关系（r=0.999 9），罗红霉素片平均回收率99.6%（RSD=0.8%）;罗红霉素分散片平均回收率99.4%（RSD=0.9%）。17批片剂和13批分散片在45 min时平均溶出量均＞80%,且均一性较好。结论该方法快速、简便，结果准确可靠，重复性好。     

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.     

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.     

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.