高效液相色谱法测定莲胆消炎片中穿心莲内酯和脱水穿心莲内酯含量

目的建立测定莲胆消炎片中穿心莲内酯和脱水穿心莲内酯含量的高效液相色谱法。方法采用Agilent C18柱（150 mm×4.6 mm,5μm）;甲醇-水（52∶48）为流动相。穿心莲内酯的流量为0.8 mL/min,检测波长为225 nm;脱水穿心莲内酯的流速为0.8 mL/min,检测波长为254 nm;柱温30℃;进样量为10μL。结果莲胆消炎片中穿心莲内酯和脱水穿心莲内酯的进样量均在5～400μg范围内与峰面积呈良好线性关系,r=0.999 9（n=5）,平均回收率为97.74%。结论该方法快速、简便、灵敏、准确,适合于莲胆消炎片中穿心莲内酯和脱水穿心莲内酯的含量测定。     

HPLC测定莲芝消炎片中穿心莲内酯和脱水穿心莲内酯的含量

目的建立莲芝消炎片中穿心莲内酯和脱水穿心莲内酯的含量测定方法。方法采用HPLC法,色谱柱为C18柱,以甲醇-水(52∶48)为流动相,穿心莲内酯检测波长为225nm,脱水穿心莲内酯检测波长为254nm。结果穿心莲内酯和脱水穿心莲内酯的线性范围分别为0.0810～0.810mg.L-1(r=0.9997)和33.16～331.6mg.L-1(r=0.9995),回收率分别为97.2%(RSD为1.6%)和96.5%(RSD为2.0%)。结论方法简便可靠,重现性好,可控制其质量。     

HPLC法测定莲芝消炎胶囊中穿心莲内酯和脱水穿心莲内酯的含量

目的:建立反相高效液相色谱法测定莲芝消炎胶囊中穿心莲内酯和脱水穿心莲内酯含量的方法。方法:色谱柱为Kromasil-C_(18)柱(250 mm×4.6 mm,5μm),流动相为甲醇-水(55:45),流速1.0ml·min~(-1),检测波长225 nm,柱温40℃。结果:穿心莲内酯在0.23～2.30μg范围内线性良好。r=0.999 8,平均加样回收率为100.40%,RSD 为2.13%;脱水穿心莲内酯在0.25～2.50μg范围内线性良好,r=0.999 8,平均加样回收率为101.8%,RSD 为2.0%。结论:该方法简便、准确、灵敏度高,可有效控制莲芝消炎胶囊的质量。     

高效液相色谱法测定穿黄消炎片中穿心莲内酯和脱水穿心莲内酯的含量

目的建立HPLC测定穿黄消炎片中穿心莲内酯和脱水穿心莲内酯含量的方法。方法色谱柱为Dikma Di-amonsil C18柱(4.0 mm×250 mm,5μm),以甲醇-水(50∶50)为流动相,脱水穿心莲内酯检测波长254 nm、穿心莲内酯检测波长为225 nm;采用外标法定量。结果穿心莲内酯与脱水穿心莲内酯的线性范围内分别为2.928~146.4μg.mL-1和5.98~299μg.mL-1,相关系数r均为0.999 9;回收率分别为101.82%(RSD=2.2%)和97.52%(RSD=2.4%)。结论本方法操作简便、重现性好,适合于本制剂的含量测定。     

莲芝消炎片的质量标准研究

目的:建立莲芝消炎片的质量控制标准。方法:采用薄层色谱(TLC)法对莲芝消炎片中穿心莲、山芝麻进行定性鉴别,采用高效液相色谱法对莲芝消炎片中的脱水穿心莲内酯进行含量测定。结果:TLC斑点清晰、分离度好,阴性对照无干扰;脱水穿心莲内酯进样量在0.516～5.16μg范围内与峰面积积分值呈良好线性关系(r=0.9999),平均回收率为98.46%,RSD=2.89%(n=6)。结论:所建标准可用于莲芝消炎片的质量控制。     

HPLC法测定清火栀麦片中穿心莲内酯、脱水穿心莲内酯的含量

目的建立用HPLC法测定清火栀麦片中穿心莲内酯、脱水穿心莲内酯的含量。方法采用C18柱(250mm×4.6mm5μm);以甲醇-水(55:45)为流动相,穿心莲内酯检测波长为230nm;脱水穿心莲内酯检测波长为250nm,流速:1.0mL·min-1。结果穿心莲内酯在4.02-32.16μg呈良好的线性关系(r=0.9999),回收率为98.8%,RSD为0.37%(n=6);脱水穿心莲内酯在4.12-32.96μg范围内呈良好的线性关系(r=0.9999),回收率为98.8%,RSD为0.38%(n=6)。结论本法快速、准确,可同时测定清火栀麦片中穿心莲内酯、脱水穿心莲内酯的含量。     

HPLC法测定清咽胶囊中穿心莲内酯和脱水穿心莲内酯的含量

目的建立清咽胶囊中穿心莲内酯和脱水穿心莲内酯的含量测定方法。方法应用HPLC法,选用R eliesil C18色谱柱(250×4.6mm,5μm),流动相为甲醇-水(65∶35),流速为:1m.lm in-1,检测波长为250nm。结果本品中穿心莲内酯含量测定线性范围为0.084~0.756μg(r=0.9999),平均回收率为97.5%(RSD=2.26%,n=5);脱水穿心莲内酯含量测定线性范围为0.036~0.324μg(r=0.9998),平均回收率为100.1%(RSD=0.86%,n=5)。结论含量测定方法准确可行,重复性好,作为药品标准可有效地控制清咽胶囊的质量。     

双波长HPLC法同时测定穿心莲浸膏中穿心莲内酯和脱水穿心莲内酯的含量

目的建立双波长高效液相色谱法同时检测穿心莲浸膏中穿心莲内酯和脱水穿心莲内酯的含量测定方法。方法采用Intersil C18色谱柱（250 mm×4.6 mm,5μm）,以甲醇—水（60∶40）为流动相;检测波长穿心莲内酯为225 nm,脱水穿心莲内酯为254 nm;柱温为35℃;流速为1.0 mL·min-1。结果穿心莲内酯进样量在0.1043～1.0430μg范围内与峰面积呈良好的线性关系（r=1.000 0,n=5）,脱水穿心莲内酯进样量在0.099 9～0.999 0μg范围内与峰面积呈良好的线性关系（r=1.000 0,n=5）;穿心莲内酯的平均加样回收率为98.53%（RSD=1.27%,n=6）,脱水穿心莲内酯的平均加样回收率为101.51%（RSD=1.10%,n=6）。结论该方法灵敏度高,重现性好,能准确测定穿心莲浸膏中穿心莲内酯和脱水穿心莲内酯的含量。     

穿心莲药材及其制剂中6个内酯类成分的含量分析

目的:建立RP-HPLC法同时测定穿心莲药材及其制剂中6个主要内酯成分(穿心莲内酯、异穿心莲内酯、新穿心莲内酯、去氧穿心莲内酯、脱水穿心莲内酯和穿心莲宁)的含量。方法:采用Kromasil RP-C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-水为流动相,采用二元梯度洗脱,流速1.0 mL.min-1,检测波长226 nm,柱温25℃。结果:穿心莲内酯、异穿心莲内酯、新穿心莲内酯、去氧穿心莲内酯、脱水穿心莲内酯和穿心莲宁的线性范围分别为0.17～6.72μg(r=0.9970),0.04～1.67μg(r=0.9967),0.11～4.32μg(r=0.9964),0.11～4.32μg(r=0.9969),0.19～7.60μg(r=0.9965),0.03～1.24μg(r=0.9972);穿心莲药材平均加样回收率(n=6)分别为100.5%(RSD=2.3%),100.7%(RSD=2.9%),99.3%(RSD=2.1%),100.8%(RSD=3.0%),100.9%(RSD=3.0%),101.3%(RSD=2.7%)。结论:所建立的含量测定方法简便可行,重复性良好,可用于穿心莲药材及...     

HPLC法测定穿心莲滴丸中穿心莲内酯和脱水穿心莲内酯的含量

目的建立测定穿心莲内酯和脱水穿心莲内酯总含量的方法,用于穿心莲滴丸的质量控制。方法采用HPLC法。色谱柱:Diamonsil ODS柱(4.6 mm×250 mm,5μm),流动相:甲醇-水(体积比60∶40),流速:1.0 mL.min-1,检测波长:231 nm,柱温:35℃。结果穿心莲滴丸中穿心莲内酯、脱水穿心莲内酯与其他成分分离良好;穿心莲内酯的质量浓度在50.0~300.0 mg.L-1(r=0.999 8)内、脱水穿心莲内酯的质量浓度在20.0~120.0 mg.L-1(r=0.999 7)内与峰面积呈现良好的线性关系;穿心莲内酯、脱水穿心莲内酯的回收率分别为101.62%、97.72%,RSD分别为1.9%、2.1%。结论该方法可有效地控制穿心莲滴丸的质量。     

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.