改进HPLC柱切换法血浆直接进样测定法莫替丁

建立了以ＲＰ２为预处理柱，水为预处理流动相，以０．２ｍｏｌ／Ｌ乙酸和０．２ｍｏｌ／Ｌ乙酸铵为净化精洗液，血浆直接进样，在线固相浓缩净化样品，以Ｓｈｉｍｐａｃｋ ＣＬＣ－ＯＤＳ为分析柱，甲醇－乙酸胺为分析流动相，２６７ｎｍ波长检测，外标法定量测定人体血浆中法莫替丁的浓度的方法。     

诺氟沙星的HPLC测定

以高效液相色谱法测定诺氟沙星的含量，采用岛津ＳｈｉｍｐａｃｋＣＬＣ－ＯＤＳ色谱柱、０．０５ｍｏｌ／Ｌ柠檬酸－１ｍｏｌ／Ｌ乙酸铵－乙腈（７９：１：２０）为流动相，ＵＶ检测波长２７８ｎｍ，按外标法计算。本法专属性高，结果满意。     

HPLC柱切换法对炔诺酮α，β－聚（3－羟丙基）－DL－天冬酰胺在兔体内释放炔诺酮的测定

以柱切换ＨＰＬＣ（ＣＳＨＰＬＣ）技术，对炔诺酮α，β－聚（３－羟丙基）－ＤＬ天冬酰胺在家兔体内释放液中炔诺酮的血药浓度进行了测定，以自制ＯＤＳ预柱，水为流动相联机净化、富集样品；以Ｓｈｉｍ－ｐａｃｋＣＬＣ－ＯＤＳ为分析柱，甲醇－水（７：３）为流动相。结果表明ＣＳＨＰＬＣ对炔诺酮血药浓度有良好的选择性，回收率为８２．６％（ｎ＝５），日内和日间精密度（ＲＳＤ）分别小于４％和６％。在血清０．２２～１．１０μｇ／ｍ１范围内炔诺酮色谱峰面积与浓度有较好的线性关系（ｎ＝５，ｒ＝０．９９８）．     

维多宝泡腾片中泛酸钙的HPLC测定

用ＳｈｉｍｐａｃｋＣ１８柱，乙腈－０．３ｍｏｌ／Ｌ磷酸二氢钾（８∶９２，磷酸调节ｐＨ３．０）为流动相，采用ＨＰＬＣ法测定维多宝泡腾片中泛酸钙的含量，平均回收率为９９．７％，ＲＳＤ为０．８０％。     

RP─HPLC法测定兔血浆中安乃近及其活性代谢物的浓度

本文以２－萘磺酸钠为内标，建立了ＲＰ－ＨＰＬＣ法测定兔血浆中安乃近及其３种活性代谢物ＦＡＡ、ＡＡ、ＭＡＡ的浓度。Ｓｈｉｍ－ＰａｃｋＣＬＣ－ＯＤＳ（１５ｃｍ×６ｍｍＩＤ）为分析柱；ＯＤＳ预柱；流动相组成：甲醇－水－０．５ｍｏｌ／Ｌ磷酸二氢钠－三乙胺（３５：６３：２：０．０１），磷酸调节ｐＨ６．０±０．５；流速：１．０ｍｌ／ｍｉｎ；柱温：３５℃；检测彼长：２６０ｎｍ。本法简便、快速、准确、灵敏，适用于安乃近及其活性代谢物的血药浓度测定及药物动力学研究。     

氨甲环酸中顺式异构体的高效液相色谱法测定

本文采用高效液相色谱法测定氨甲环酸中的顺式异构体含量。先用衍生化试剂３，５－二硝基苯酰氯预处理氨甲环酸，然后通过ＨＰＬＣ，以喹啉为内标，ＹＭＣ－ＰａｃｋＡＭ－３０２ＯＤＳ为色谱柱，甲醇－０．０２ｍｏｌ／Ｌ醋酸铵溶液（４：７）为流动相，在２５４ｎｍ波长处检测，顺式异构体在１～２．５μｇ／ｍｌ范围内线性关系良好（ｒ＝０．９９６１），最低检测限为０．０２％。     

小儿镇咳合剂中磷酸可待因的HPLC测定

在碱性溶液中经加盐和氯仿提取后采用ＨＰＬＣ法，用Ｓｈｉｍ－Ｐａｃｋ，ＣＬＣ－ＯＤＳＣ１８柱，以０．０１ｍｏｌ／Ｌ溴化四甲基铵溶液（ＨＯＡｃ调节ｐＨ＝３）－甲醇（４２∶５８）为流动相，能使小儿镇咳合剂中磷酸可待因得到很好的分离。平均回收率为１００．１％，ＲＳＤ为０．９５％。     

对乙酰氨基酚中对氯乙酰苯胺的限量分析

以Ｎｏｖａ－ＰａｃｋＣ１８为色谱柱，０．０１ｍｏｌ／Ｌ庚烷磺酸钠－甲醇－甲酸（８５１５０．５）为流动相，检测波长２５４ｎｍ，采用ＨＰＬＣ法测定对乙酰氨基酚中对氯乙酰苯胺的限量     

复方胶囊中右美沙芬和布落芬的溶出度测定

用ＨＰＬＣ测定复方胶囊中右美沙芬、布洛芬的溶出度。色谱柱为Ｓｈｉｍｐａｃｋ ＣＬＣ－ＯＤＳ柱,流动相为乙脯－水（６５：３５含０．００７ｍｏｌ／Ｌ硝酸铵、０．００７ｍｏｌ／Ｌ ＳＤＳ,用冰醋酸调ＰＨ至３．４）,流速１．０ｍｌ／ｍｉｎ,在２７０ｎｍ处测定。右美沙芬、布洛芬的线性范围分别为５～４０,５０～４００μｇ／ｍｌ。两者的平均回经分别为９９．２６％、９９．７０％。     

高效液相色谱法测定中药复方制剂中黄芩甙的含量

本文建立了一种中药复方制剂中黄芩甙含量的ＨＨＰＬＣ测定方法。ＳｈｉｍｐａｃｋＣＬＣ－ＯＤＳ（１５０ｍｍ×６ｍｍｉ．ｄ．），流动相为甲醇：０．２ｍｏｌ／Ｌ磷酸二氢钠（ｐＨ２．７）（５０：５０），检测波长为２７５ｎｍ，柱温３５℃，黄芩甙保留时间约为１６．５ｍｉｎ。本文分离效果佳，回收率和精密度均好，适于制剂生产中的质量控制。     

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.     

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.