RP-HPLC法同时测定补肾益脑胶囊中五味子醇甲、五味子甲素和五味子乙素的含量

目的建立用RP-HPLC(反相高效液相色谱)法同时测定补肾益脑胶囊中五味子醇甲、五味子甲素和五味子乙素含量的方法。方法色谱柱为Agilent C18,流动相为甲醇-水(70∶30),检测波长为250nm,流速为0.8mL·min-1,进样量为10μL。结果五味子醇甲、五味子甲素和五味子乙素进样浓度的线性范围分别为10.17～203.37μg·mL-1(r=0.9997)、2.17～43.43μg·mL-1(r=0.9997)、2.82～56.40μg·mL-1(r=0.9995),平均回收率分别为97.9%(RSD=1.45%,n=9)、98.7%(RSD=1.71%,n=9)、97.4%(RSD=1.56%,n=9)。结论本方法结果准确,重复性好,可用于补肾益脑胶囊的质量控制。     

反相高效液相色谱法测定参松养心胶囊中五味子甲素和五味子酯甲含量

目的建立高效液相色谱法测定参松养心胶囊中五味子甲素和五味子酯甲含量的方法。方法采用RP-HPLC法,色谱柱：Agilent Extend C18（250mm×4.6mm,5μm）;流动相：乙腈-水,梯度洗脱;流速：1.0mL.min-1;检测波长：230nm;柱温：35℃。结果五味子甲素进样量在0.020 2～0.161 7μg与峰面积线性关系良好,r=0.999 5,平均加样回收率为100.8%,RSD=0.3%;五味子酯甲进样量在0.021 0～0.168 0μg与峰面积线性关系良好,r=0.999 6,平均加样回收率为101.8%,RSD=0.3%。结论所建立的含量测定方法简便可行,结果准确可靠,可用于参松养心胶囊中五味子甲素和五味子酯甲的含量测定。     

HPLC法同时测定参芪五味子胶囊中五味子酯甲和五味子甲素的含量

目的:建立同时测定参芪五味子胶囊中五味子酯甲和五味子甲素含量的方法。方法:采用高效液相色谱法。色谱柱为Waters Xterra Ms C18,流动相为乙腈-四氢呋喃-水(18∶18∶64,V/V/V),流速为1.0 ml/min,检测波长为222 nm,柱温为25℃,进样量为10μl。结果:五味子酯甲和五味子甲素进样量分别在0.026 2⁰.418 4、0.024 90.418 4、0.024 9⁰.398 4μg范围内与各自峰面积积分值呈良好的线性关系(均r=0.999 9);精密度、稳定性、重复性试验的RSD≤1.7%;平均加样回收率分别为101.1%、100.8%,RSD分别为1.6%、1.5%(n=9)。结论:该方法重复性好、灵敏度高、结果准确可靠,可用于参芪五味子胶囊的质量控制。     

HPLC切换波长法同时测定参芪五味子片中五味子酯甲和五味子甲素的含量

目的通过切换波长高效液相色谱法同时测定参芪五味子片中五味子酯甲和五味子甲素的含量。方法采用高效液相色谱法,使用Agilent Zorbax SB-C18(250 mm×416 mm,5μm)色谱柱,以甲醇-水(69∶31)为流动相,流速:1.0 mL.min-1,柱温:40℃,五味子酯甲检测波长为222 nm,五味子甲素检测波长为251 nm。结果五味子酯甲、五味子甲素分别在0.171~3.420μg(Y=24 107 309X+2.717 84×105,r=0.999 9),0.218~5.460μg(Y=2 069 343X+1.041 10×105,r=0.999 9)范围内与峰面积呈良好的线性关系。平均加样回收率分别为99.73%,99.21%,RSD(n=6)分别为1.3%,1.4%。结论本法灵敏、准确、简便、快速,可用于同时测定参芪五味子片中五味子酯甲和五味子甲素含量。     

RP-HPLC 法测定舒神灵胶囊中五味子醇甲的含量

目的 建立舒神灵胶囊中五味子醇甲的含量测定方法.方法 采用RP-HPLC法,以甲醇-水(63:37)为流动相;检测波长为250nm.结果 五味子醇甲在10.24～153.60μg/ml(r=1.0000)范围内线性关系良好;平均回收率为99.85 %,RSD 为0.54%(n=6).结论 RP-HPLC法简便可靠,专属性强,重现性好,可用于舒神灵胶囊的质量控制.     

高效液相色谱法测定北五味子藤茎超临界提取物中五味子甲素、五味子乙素和五味子醇甲的含量

目的 高效液相色谱(HPLC)法测定北五味子藤茎超临界提取物中五味子甲素、五味子乙素、五味子醇甲的含量.方法 采用ODS-C18(5 μm,4.6 × 250 mm),以甲醇-水(75:25)为流动相,流速:1.0 ml/min,检测波长为254 nm.结果 五味子甲素、五味子乙素、五味子醇甲的线性范围分别为0.1～2.0μg/(r=0.9994)、0.1～2.0μg(r=0.9997)、0.12～2.0μg(r=0.9992),平均加样回收率分别为99.03%、103.60%、99.80%,RSD分别为1.72%、2.09%、1.33%(n=5).结论 本方法简便准确、重现性好,能有效测定北五味子藤茎超临界提取物中五味子甲素、五味子乙素、五味子醇甲的含量.     

五味子降酶胶囊质量控制研究

目的 探讨五味子降酶胶囊的质量控制方法.方法 采用薄层色谱法(TLC)鉴别五味子降酶胶囊中的五味子、板蓝根;采用高效液相色谱法(HPLC)测定五味子中五味子醇甲的含量.结果 薄层鉴别斑点清晰,分离效果好,专属性强;含量测定中五味子醇甲在0.03337～0.53392μg范围内,与峰面积线性关系良好(r=0.9995)....     

反相高效液相色谱法测定复方五仁醇胶囊中2组分的含量

目的建立以反相高效液相色谱法测定复方五仁醇胶囊中五味子醇甲和五味子乙素含量的方法。方法色谱柱为Lichro-sphereC18,流动相为水-甲醇(梯度洗脱),流速为1.0mL.min-1,柱温为30℃,检测波长为254nm。结果五味子醇甲、五味子乙素进样量分别在0.1824~1.6416μg(r=1.0003)、0.1896~1.7064μg(r=0.9999)范围内与峰面积积分值线性关系良好;平均加样回收率分别为98.32%(RSD=1.02%)、97.22%(RSD=0.94%)。结论本方法简便、准确、专属性强,可用于本品的质量控制。     

五香血藤中五味子醇甲与五味子甲素含量测定

目的建立同时测定五香血藤中五味子醇甲与五味子甲素含量的高效液相色谱法。方法采用反相高效液相色谱法,C18色谱柱(4.6 mm×250 mm,5μm),乙腈(A)-水(B)为流动相,梯度洗脱,流速1 mL.min-1,五味子醇甲检测波长216 nm,五味子甲素检测波长209 nm。结果五味子醇甲在0.019 6～0.215 6μg之间线性关系良好,回收率99.11%,RSD=2.02%(n=9);五味子甲素在0.018 4～0.147 2μg之间线性关系良好,回收率102.35%,RSD=1.73%(n=9)。结论该方法简便、准确,可用于五香血藤中五味子醇甲与五味子甲素的含量测定。     

RP-HPLC法测定复方五味子胶囊中五味子甲素的含量

目的建立测定复方五味子胶囊中五味子甲素含量的高效液相色谱法。方法采用Kro-masilC18（250mm×4.6mm,5μm）的色谱柱;以甲醇-0.1%冰醋酸水溶液（82∶18）为流动相;流速：1ml/min;检测波长：254nm;柱温为30℃。结果五味子甲素在0.1137～0.4547mg/ml范围内与峰面积呈良好的线性关系（r=0.9992,n=6）,平均加样回收率为99.01%（RSD=1.1%,n=6）。结论HPLC法测定复方五味子胶囊中五味子甲素含量方法简便、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.     

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.     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

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.