当归、川芎中藁本内酯含量测定及醇提工艺研究

目的研究当归、川芎中藁本内酯醇提的最佳工艺条件。方法建立HPLC法测定提取液中指标成分藁本内酯的含量 ,并用正交设计优化醇提工艺条件。结果与结论用甲醇 - 水 - 乙酸(V∶V∶V =75 . 0∶2 4 . 8∶0 . 2 )作流动相能使藁本内酯得到良好的分离 ;8倍量 85 % (φ)乙醇提取3次 ,每次 1 0h为醇提最佳工艺条件。     

川芎化学成分分离鉴定与藁本内酯的含量测定

目的:分离并鉴定川芎有效部位的化学成分,建立川芎药材中藁本内酯的含量测定方法。方法:采用乙醇渗漉提取、硅胶柱色谱分离,运用1H-NMR、13C-NMR鉴定化合物结构;采用高效液相色谱(HPLC)法测定藁本内酯的含量。结果:共分离鉴定了3个化合物,分别为Z-藁本内酯、Z-6,8′,7,3′-二聚藁本内酯、Z,Z′-6,6′,7,3′a-二聚藁本内酯;药材中藁本内酯含量不低于0.70%。结论:本试验建立的分离方法可用于制备藁本内酯标准品,含量测定方法可用于川芎药材的质量控制。     

双波长薄层扫描法测定当归散中藁本内酯的含量

目的 :建立当归散中藁本内酯的测定方法。方法 :双波长薄层扫描法 (λs=2 90nm ,λR=370nm)。结果 :藁本内酯在 5～ 2 5 μg线性关系良好 ,γ =0 .9986 ,平均回收率为 96 .9% ,RSD为 1.49% (n =5 )。 3批样品含量分别为 0 .332 ,0 .35 4,0 .32 3mg·g-1。结论 :本法简便、准确 ,可作为当归散中藁本内酯的测定方法。     

HPLC法同时测定当归药材中6种成分的含量

目的:建立高效液相色谱法同时测定当归药材中阿魏酸、阿魏酸松柏酯、Z 型和 E 型藁本内酯及 Z 型和 E 型3-丁烯基苯酞的含量。方法:采用 Zorbax ODS C_(18)色谱柱(250 mm×4.6 mm,5 μm);流动相为1%醋酸(A)-乙腈(B),梯度洗脱(0min,10%B;7 min,33%B;55 min,33%B),流速1.0 mL·min~(-1);检测波长为324 nm(阿魏酸、阿魏酸松柏酯和 Z/E 型藁本内酯)和260 nm(Z 型和 E 型3-丁烯基苯酞)。结果:阿魏酸、阿魏酸松柏酯、Z-藁本内酯、Z 型和 E 型3-丁烯基苯酞的线性范围分别为3.31～139.50 μg·mL~(-1)(r=0.9999),38.00～380.00 μg·mL~(-1)(r=0.9995),2.11～445.00 μg·mL~(-1)(r=1.000),3.32～136.18 μg·mL~(-1)(r=0.9999),1.94～16.32 μg·mL~(-1)(r:0.9995);加样回收率分别为101.8%(RSD=2.5%),105.3%(RSD=3.2%),98.5%(RSD=1.6%),105.3%(RSD=2.4%),105.8%(RSD=1.9%)。结论:该方法准确、简便,具有良好的重复性和稳定性,有利于提高当归药材的质量控制。     

HPLC法同时测定胃痛欣颗粒剂中大黄酸、大黄素、大黄酚的含量

目的建立胃痛欣颗粒剂中大黄酸、大黄素、大黄酚的含量测定方法。方法采用高效液相色谱法 ,AccusilC1 8(4 6mm× 2 5 0mm ,1 0 μm)柱 ,流动相为 :甲醇 水 冰醋酸 (80∶2 0∶1 ,V∶V∶V) ,检测波长为 2 5 4nm。结果大黄酸、大黄素、大黄酚分别在 0 0 3～ 0 4 8μg ,0 0 2 5～ 0 4 0 μg ,0 0 2 5～0 4 0 μg内与峰面积呈线性关系 ,平均回收率 (n =3 )分别为 98 3 % (RSD =1 4 3 % ) ,97 6% (RSD=1 84 ) ,98 7% (RSD =0 5 7% )。结论可用于大黄药材及其复方制剂的质量控制     

蒸馏-萃取耦合法提取川芎挥发油及质量评价

目的:建立蒸馏-萃取耦合法提取川芎挥发油新工艺和藁本内酯含量测定方法。方法:优选蒸馏-萃取耦合法提取川芎挥发油新工艺,气相色谱程序升温法测定藁本内酯含量。结果:确定了最佳提取工艺为以1.5 ml液体石蜡为萃取剂,用乙醇和20%的NaCl水溶液萃取分离得到川芎挥发油;建立了川芎挥发油中藁本内酯含量气相色谱测定法,藁本内酯在121.09~1 009.10 mg·ml^-1范围内线性关系良好,平均回收率为99.30% (n=9)。结论:所建立的蒸馏-萃取耦合法提取川芎挥发油的新工艺优于川芎挥发油的传统蒸馏法,其含量测定方法可用于川芎挥发油中藁本内酯的含量测定。     

紫外分光光度法测定川芎油中的总内酯

目的 采用紫外分光光度测定川芎油中的总内酯.方法 以藁本内酯作对照品,样品和对照品中加入4 ml 30 mg·ml-1的NaOH溶液,30℃保温反应30 min后,于305 nm测定吸光度.结果 藁本内酯2.95～23.6 μg·ml-1与吸光度呈良好的线性关系,其同归方程为:Y=36.8X+0.009(r=0.9998),总内酯的平均回收率为98.1%,RSD=1.1%.3批川芎油含量测定的结果分别为51.3%、53.0%、57.5%.结论 所建方法可以作为川芎油中总内酯的含量测定方法.     

HPLC法同时测定川芎药材中阿魏酸和藁本内酯的含量

目的:建立高效液相色谱法同时测定川芎药材中阿魏酸和藁本内酯的方法。方法:采用Dikma Kromasil C18(250 nm×4.6 mm,5μm)色谱柱;流动相为甲醇-0.1%冰醋酸水溶液(65∶35);流速1.0 mL.min-1;检测波长:320nm;柱温30℃。结果:川芎药材中2种成分得到良好的分离,阿魏酸在0.032~0.3179μg范围内,藁本内酯在0.244~2.44μg范围内线性关系良好,平均回收率分别为98.4%和98.8%。结论:本方法简便,准确,重复性好,为多组分评价川芎药材质量提供了可靠的分析方法。     

RP-HPLC法测定野菊花中蒙花苷含量

目的建立野菊花中蒙花苷的含量测定方法。方法采用反相高效液相色谱法 ,DiamonsilTMC18柱 (2 5 0mm× 4 6mm ,5 μm) ,流动相为甲醇 水 磷酸 (体积比 5 7∶4 3∶0 0 4 ) ,检测波长为32 6nm。结果蒙花苷线性范围 0 4 8～ 9 70mg·L-1,r =0 9999(n =7) ;平均回收率为 98 4 % ,RSD为 2 0 % (n =9)。结论该测定方法为野菊花药材的质量控制提供依据     

复方藁本内酯微乳的制备和含量测定

目的:制备复方藁本内酯微乳并测定其主要成分藁本内酯和桂皮醛的含量.方法:制备复方藁本内酯微乳,HPLC法测定其主要成分含量.色谱柱为Inertsil ODS-3 (250 mm×4.6 mm,5μm).测定藁本内酯时流动相为乙腈∶甲醇∶水(10∶60∶30),柱温为5℃,检测波长为280 nm;测定桂皮醛时流动相为甲醇∶水(60∶ 40),柱温为25℃;检测波长为290 nm.流速均为1.0 ml·min-1.结果:藁本内酯在0.50 ～50.00 μg·ml-1(r =0.999 9),桂皮醛在1.30 ～130.18 μg· ml-1(r =0.999 8)范围内线性良好,藁本内酯的回收率为99.65％,RSD为0.97％(n=9);桂皮醛的回收率为99.81％,RSD为0.62％(n=9).结论:复方藁本内酯微乳制备简单,以HPLC方法测定其主成分含量快速,准确,可靠.     

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.