荧光分光光度法测定何首乌及人参首乌胶囊中总葸醌的含量

目的：建立测定何首乌及人参首乌胶囊中总蒽醌含量的方法。方法：荧光分光光度法。以最佳pH条件的无水乙醇为溶剂，在λEX=440nm、λEM=515nm处测定总蒽醌含量。结果：在0．03～0．15p,g·mL^-1范围内，大黄素浓度和荧光强度有良好的线性关系，回归方程为F=194．36C＋2．9642，r=0．9996。平均回收率何首乌为98．1％，RSD为1．9％；人参首乌胶囊为98．6％，RSD为2．0％。测得总蒽醌含量何首乌中为0．522mg·g^-1，人参首乌胶囊中为0．443mg·g^-1。结论：本法简便快捷，准确灵敏，重复性好，可用于何首乌及人参首乌胶囊的质量控制。     

HPLC同时测定不同何首乌中的两种蒽醌类成分

目的 比较生何首乌、制何首乌及其发酵产品中游离型和结合型蒽醌类成分的含量.方法 采用HPLC法测定了不同何首乌蒽醌中两者的含量.色谱柱为Diamonsil C18(150 mm×4.6 mm,5 μm)柱,流动相为乙腈-0.1%磷酸(70:30),检测波长为254 nm,流速为1.0 ml·min-1.结果 大黄素、大黄素甲醚的线性范围分别为0.02～0.40 μg (r=0.9994)、0.01～0.20μg(r=0.9994),游离大黄素与大黄素甲醚测定的平均回收率分别为99.9%(RSD=1.9%)、97.9%(RSD=1.5%),总大黄素与大黄素甲醚的平均回收率分别为95.8%(RSD=3.7%)、105.9%(RSD=2.2%).结论 何首乌经炮制和发酵后,结合型蒽醌的含量明显低于生何首乌,文中方法准确可靠,可用于何首乌的质量控制.     

差示比色法测定润肠胶囊中游离羟基蒽醌的含量

目的建立差示比色法测定润肠胶囊中游离羟基蒽醌的含量。方法以1%醋酸镁甲醇溶液为显色剂,于516 nm波长处测定羟基蒽醌-醋酸镁络合物与其他非蒽醌类醇溶物的吸收差ΔA,代入标准曲线方程A(ΔA)=0.048 24C-0.008 6计算游离羟基蒽醌的含量。结果平均回收率为98.07%±1.08%,RSD=1.09%,在5~15mg.L-1线性关系良好(r=0.999 8)。结论本方法准确,精密度好,操作易掌握,可用于芦荟、何首乌等中药及其制剂中的游离羟基蒽醌含量测定。     

荧光猝灭法测定盐酸胺碘酮含量

目的:建立荧光猝灭法测定盐酸胺碘酮片剂含量的新方法。方法:试验多种荧光试剂加入系列浓度的胺碘酮溶液,测定其荧光光谱的变化。结果:选用芘丁酸(PBA)为荧光试剂,浓度为2.0mg·L~(-1),λ_(ex)/λ_(em)=349nm/376.3nm,在2.0～20mg·L~(-1)胺碘酮浓度范围与荧光猝灭值(F_0/F)成良好的线性关系(r=0.9962),据此提出测定片剂中胺碘酮含量的荧光猝灭法。结论:荧光猝灭法简便灵敏、选择性高,可用于药片中盐酸胺碘酮含量的测定。     

人参首乌胶囊中人参皂苷Rg1的含量测定

目的建立人参首乌胶囊中人参皂苷Rg1的含量测定方法。方法采用高效液相色谱（HPLC）法。固定相为kromasailC18柱,流动相为乙腈-0.05%磷酸溶液（19：81）,紫外检测波长203nm。结果人参皂苷Rg1在0.0524～0.524mg/ml范围内线性关系良好,r=0.9999（n=5）;平均加样回收率为96.86%（n=9）,RSD=1.19%。结论该方法简便、快捷、准确,可用于人参首乌胶囊中人参皂苷Rg1的含量测定。     

分光光度法测定益气胶囊中总皂苷含量

目的:建立益气胶囊中人参总皂苷含量的测定方法。方法:采用大孔吸附树脂分离-比色法测定,以香草醛-硫酸为显色剂,人参皂苷Rg1为对照品,测定波长λ=542 nm。结果:人参皂苷Rg1在0.049～0.194 mg/mL浓度范围内线性关系良好,Y=5.7356X-0.176,r=0.9990。平均回收率为96.95%±1.29%,方法精密度RSD=2.97%(n=5)。测得4批样品的标示量分别为0.24%、0.23%、0.28%、0.27%。结论:本方法简便、快速、准确、重复性好,可用作益气胶囊的质量控制。     

薄层扫描法测定益康胶囊中人参皂苷Re的含量

采用薄层扫描法测定益康胶囊中人参皂苷 Re的含量 :λS=5 75 nm,λR=5 2 2 nm。试样先经氯仿处理、甲醇提取 ,再经氯化铝柱层析 ,正丁醇萃取 ,平均回收率 96.1 5 % ,RSD =1 .2 0 %。 3批益康胶囊中人参皂苷 Re含量分别为 0 .5 34mg/g,0 .486mg/g,0 .5 0 0 mg/     

高效液相色谱荧光检测法测定人血浆中替米沙坦浓度及其应用

目的:建立高效液相色谱荧光检测人血浆中替米沙坦浓度的方法,并用于研究替米沙坦片的人体药代动力学。方法:采用固相萃取方法提取血浆中的替米沙坦,色谱柱为 Diamonsil C_(18)柱(5μm,4.6mm×150mm),以乙腈-磷酸二氢钾缓冲液(61∶39,磷酸调 pH=3.74)为流动相,流速1.0mL·min~(-1),坎地沙坦为内标,荧光检测波长λ_(Ex)=305nm,λ_(Em)=365nm。结果:本法测定替米沙坦的线性范围为0.5-144ng·mL~(-1),r=0.9998,绝对回收率在79.62%-85.69%(n=5),相对回收率在101.9%-109.0%(n=5),日内和日间 RSD 分别为4.23%-9.80%和4.03%-9.95%(n:5)。结论:本法灵敏、准确,操作简捷,适用于替米沙坦的血药浓度测定及药代动力学研究。     

高效液相色谱-荧光检测法测定红景天苷的含量

目的:建立高效液相色谱-荧光检测法测定红景天苷的含量。方法:色谱柱为 Eclipse XDB-C_8柱(4.6 mm × 150 mm,5μm),流动相为水-甲醇(85:15),流速为1.0 mL·min~(-1),柱温为25℃,荧光检测波长λ_(EX)=220 nm,λ_(EM)=315 nm。结果:该方法的线性范围为1.00～500 ng(r=0.999 9)。平均加样回收率为 99.2％,RSD为 1.4％(n=5)。最低检测限为1.5 pg。结论:本方法快速,简单,灵敏度极高。     

真人妇科宝胶囊质量控制研究

建立了真人妇科宝胶囊中当归、川芎、延胡索、白术、木香薄层鉴别方法 ;探索了薄层扫描法测定胶囊中人参皂苷 Rg1含量的方法 ;结果表明试品需经乙醚脱脂 -甲醇提取 -氧化铝 -大孔树脂混和柱精制 ,双波长反射锯齿扫描定量 (λR=680 nm,λs=5 40 nm) ,回收率 98.1 3% ,RSD为 1 .5 4%。试品平均含人参皂苷 Rg10 .1 5 mg/粒     

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.