化学发光法测定山奈酚

目的:建立了流动注射化学发光测定山奈酚的分析方法。方法:在盐酸介质中,硫酸铈氧化罗丹明6G 产生弱的化学发光,山奈酚对该反应有强的增敏作用,通过测定 Ce(Ⅳ)-罗丹明6G-山奈酚体系的化学发光强度,确定样品中山奈酚的含量。结果:该方法检出限为8.5×10~(-5)μg·mL~(-1),线性范围为1×10~(-4)～1.0μg·mL~(-1),对0.05μg·mL~(-1)山奈酚进行了11次平行测定,其 RSD 为0.9%,在2 mL·min~(-1)的流速下,0.5 min 内可完成一次测定。结论:该法用于合成样品中山奈酚的测定,与紫外测定结果进行对照,无显著性差异。对化学发光可能的机理进行了讨论。     

高效液相色谱柱后化学发光检测技术对杉科植物中羟基酸的分析应用

目的:本文建立了用高效液相色谱分离柱后化学发光法测定杉科植物中羟基酸含量。方法:基于在酸性介质中高锰酸钾直接氧化酒石酸、苹果酸和莽草酸等羟基酸产生化学发光,而盐酸氨基脲能够显著增强该体系的发光强度。采用 kBPCL 超微弱发光测量仪作为检测器,Hypersil ODS(4.6mm×150mm,5μm)柱,高氯酸(pH=2.5)溶液为流动相,流速0.8mL·min~(-1)。结果:酒石酸、苹果酸和莽草酸浓度分别在8.6×10~(-7)～2.6×10~(-4)(r=0.9991),9.6×10~(-8)～3×10~(-4)(r=0.9999),2.2×10~(-7)～3.5×10~(-3)g·mL~(-1)(r=0.9998)范围内,与峰面积有良好的线性关系;检出限分别为3.54×10~(-8),2.24×10~(-9),2.02×10~(-8)g·mL~(-1)(S/N=3)。结论:该法简便、快速、有效,灵敏度高,首次用于杉科植物中羟基酸的测定,取得了很好的结果。     

用毛细管电泳电化学发光法测定盐酸氟西汀的含量

目的:在实验中观察到盐酸氟西汀能增强钌联吡啶的电化学发光信号,基此建立了一种盐酸氟西汀的毛细管电泳-电化学发光新方法。方法:在实验中,对毛细管电泳分离条件和电化学发光检测条件进行了优化。结果:在优化的实验条件下,测得盐酸氟西汀线性范围为5.0×10~(-7)～1.0×10~(-4)g·mL~(-1),检出限为5.75×10~(-8)g·mL~(-1)(S/N=3)。对1.0×10—5 g·mL~(-1)的盐酸氟西汀进行11次平行测定,峰高的相对标准偏差(RSD)为2.0%。结论:该方法可用于测定盐酸氟西汀片剂的含量。     

化学发光法快速测定盐酸托莫西汀的含量

目的:建立快速检测痕量盐酸托莫西汀的化学发光方法。方法:利用 Ce~(4 )-Na_2SO_3-H_2SO_4氧化还原体系在加入盐酸托莫西汀后发光强度明显增强的现象,建立了一种测定痕量盐酸托莫西汀的化学发光分析方法。结果:该方法的线性范围为5.0×10~(-5)～5.0×10~(-3)g·L~(-1),r=0.9991;检测限为2.0×10~(-5)g·L~(-1);RSD=2.0%(n=11)。结论:本方法快捷、简便,灵敏度高,可以用于胶囊中盐酸托莫西汀含量的测定,并与 HPLC 法进行了比较,结果满意。     

RP—HPLC法测定黄柏中小檗碱、巴马汀和药根碱的含量

目的:建立了用外标法对黄柏中小檗碱、巴马汀和药根碱同时定量的测定方法,考察小檗碱、巴马汀和药根碱的含量与其产地的关系。方法:高效液相色谱法,色谱柱:Kromasil-C_(18)(4.6mm×250mm,5μm),流动相:甲醇-乙腈-0.1mol·L~(-1)磷酸二氢钠(磷酸调pH为3.0)-2g·L~(-1)十二烷基硫酸钠-三乙胺(25∶25∶25∶25∶0.2),流速:1.0mL·min~(-1),检测波长:230nm,柱温:室温。结果:小檗碱、巴马汀和药根碱色谱峰面积与浓度呈良好的线性关系,线性范围分别是:盐酸小檗碱:21～495μg·mL~(-1),Y=3.144×10~6X 8.644×10~4,r=0.9999;盐酸巴马汀:2.0～40μg·mL~(-1),Y=7.570×10~5X 1.622×10~3,r=0.9999;盐酸药根碱:0.32～13μg·mL~(-1),Y=4.649×10~5X 2.161×10~3,r=0.9999。平均回收率小檗碱为98.0%,RSD为2.9%;巴马汀为97.7%,RSD为2.7%;药根碱为97.5%,RSD为2.4%。结论:本方法测定了21个不同产地的黄柏样品中小檗碱、巴马汀和药根碱含量,该方法分离度好,简便,重现性好。     

流动注射-化学发光法测定片剂、人血清及尿液中6-巯基嘌呤的含量

目的:研究6-巯基嘌呤-高锰酸钾-甲醛-多聚磷酸体系的化学发光行为与机理,建立流动注射-化学发光法测定片剂、人血清与尿液中6-巯基嘌呤的含量。方法:采用6-巯基嘌呤-高锰酸钾-甲醛-多聚磷酸化学发光体系,基于化学发光强度与浓度间的线性关系对6-巯基嘌呤加以定量测定。结果:校准曲线的线性范围为1.0×10~(-8)～1.0×10~(-5)g·mL~(-1),检出限为6×10~(-9)g·mL~(-1);对2.0×10~(-7)g·mL~(-1)6-巯基嘌呤进行11次平行测定,RSD 为1.7%;片剂、人血清和尿液加样回收率在95.0%～111.3%范围内,RSD 为1.8%～2.2%。结论:本方法简便、灵敏、可靠,可用于6-巯基嘌呤的常规检测及药代动力学研究。     

高效液相色谱分离柱后化学发光法同时测定菟丝子中黄酮类成分

目的:建立高效液相色谱分离柱后化学发光法测定菟丝子中芦丁、山柰素、槲皮素和异鼠李素含量。方法:基于在氢氧化钠碱性介质中铁氰化钾可以直接氧化芦丁、山柰素、槲皮素和异鼠李素产生化学发光。色谱柱:Hypersil ODS(5μm,4.6 mm×150 mm),流动相:乙醇-乙腈-水-磷酸(21:22:55:2),流速:1mL·min~(-1),柱温:25℃。结果:芦丁、山柰素、槲皮素和异鼠李素浓度分别在0.2～5μg·mL~(-1)(r=0.9990),0.1～15μg·mL~(-1)(r=0.9991),0.1～100μg·mL~(-1)(r=0.9994),0.3～200μg·mL~(-1)(r=0.9998)范围内,与峰面积有良好的线性关系;检测限(S/N=3)分别为0.02,0.08,0.08,0.03μg·mL~(-1)。结论:水法简便、快速、有效,灵敏度高,首次用于菟丝子中黄酮类成分的测定,取得了很好的结果。     

流动注射化学发光法测定吩噻嗪类药物的研究

目的:建立快速测定吩噻嗪类药物的化学发光新方法。方法:在盐酸介质中,吩噻嗪类药物能被硫酸铈氧化生成发光物质砜,从而产生化学发光。基于此,建立了吩噻嗪类药物的流动注射化学发光分析方法。结果:在优化的实验条件下,不用任何增敏剂,盐酸氯丙嗪、盐酸异丙嗪在1.0×10~(-7)～1.0×10~(-5)g·mL~(-1),奋乃静在1.0×10~(-7)～1.0×10~(-4)g·mL~(-1)范围内与化学发光强度呈良好的线性关系;检出限(3σ)分别为7.0×10~(-8)g·mL~(-1),5.0×10~(-8)g·mL~(-1),2.0×10~(-1)g·mL~(-1)。结论:本方法简便、快速、准确,灵敏度高、线性范围宽,该法应用于相应注射剂和片剂分析,结果令人满意。     

高效液相色谱法测定复方异维倍克气雾剂中异丙托溴铵和盐酸克仑特罗的含量

目的:建立高效液相色谱法测定复方异维倍克气雾剂中异丙托溴铵和盐酸克仑特罗含量。方法:采用反相高效液相色谱法。Intersil C_(18)分析色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-水(16:84;含0.4%三乙胺,磷酸调 pH 为3),流速1.5 mL·mL~(-1),检测波长205 nm。结果:异丙托溴铵和盐酸克仑特罗的理论板数分别为2400和3500。异丙托溴铵回归方程Y=128458X 58038,r=0.9999,线性范围18.20～182.0μg·mL~(-1);盐酸克仑特罗回归方程 Y=1251564X 10954,r=0.9995,线性范围9.200～46.00μg·mL~(-1)。异丙托溴铵平均回收率为97.4%(n=5),RSD 为2.2%;盐酸克仑特罗平均回收率为100.8%(n=5),RSD为1.9%。异丙托溴铵和盐酸克仑特罗最低检出浓度分别为0.2μg·mL~(-1)和0.03μg·mL~(-1)。结论:方法简便,结果准确。     

流动注射化学发光法测定盐酸麻黄碱

目的:建立灵敏的流动注射化学发光分析测定盐酸麻黄碱的方法。方法:基于盐酸麻黄碱在酸性条件下对Ce(Ⅳ)-Na2 SO3化学发光反应的增敏作用,建立了流动注射化学发光测定盐酸麻黄碱的新方法。结果:在优化的条件下,测定盐酸麻黄碱的线性范围为8.0×10-8～2.0×10-6 g.mL-1(r=0.9941),检出限为2×10-8 g.mL-1。结论:该方法简便,且有较高的灵敏度和准确度,对麻黄碱药物分析以及毒品检测都有重要的意义。     

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.