HPLC法测定腰腿痛丸中盐酸麻黄碱的含量

目的:建立用高效液相色谱(HPLC)法测定腰腿痛丸中盐酸麻黄碱含量的方法.方法:以乙腈-0.1%磷酸(9:91)为流动相,VP-ODS C18(250 mm×4.6 mm,5μm)为固定相,检测波长为207 nm.结果:盐酸麻黄碱在0.08～2.02μg的范围内线性关系良好(r=0.999 9),平均回收率为97.4%,RSD为1.9%.结论:该法快捷、简便、准确,能更好的控制其质量.     

RP-HPLC法同时测定祛风活络丸中士的宁和马钱子碱的含量

目的:建立祛风活络丸中士的宁和马钱子碱的反相高效液相分析法,为该药质量控制提供依据.方法:采用Techsphese-C18ODS色谱柱(4.6 mm×250mm,5μm);乙腈-甲醇-0.05 mol·L-1KH2PO4溶液-三乙胺(25:19:55:1,磷酸调pH至3.5)为流动相:流速1 mL·min-1;检测波长254 nm.结果:士的宁在0.3～3.6μg(r=0.999 9)、马钱子碱在0.2～2.4μg(r=0.999 6)范围内呈良好的线性关系:士的宁回收率为97.6%,RSD=2.0%;马钱子碱回收率为101.02%,RSD=1.4%.结论:本方法准确可靠,简便灵敏,重现性好,可用于祛风活络丸中士的宁和马钱子碱的质量控制.     

高效液相色谱法测定腰腿痛丸中士的宁的含量

目的:完善腰腿痛丸质量标准。方法:采用高效液相色谱法对腰腿痛丸中马钱子的主要成分士的宁进行含量测定。结果:士的宁进样量在5μg⁵0μg范围内与峰面积呈良好线性关系;平均回收率为97.68%,RSD=0.36%(n=6)。结论:完善了腰腿痛丸质量标准,该方法精确,重现性好,操作简便,可以作为腰腿痛丸质量控制标准。     

HPLC法测定肝宁丸中栀子苷的含量

目的:应用高效液相色谱法对肝宁丸中栀子苷进行含量测定.方法:选用依利特Hypersil C18分析柱(150 mm×4.6 mm,5μm),乙腈-水(11:89)为流动相,检测波长为238 nm,流速1.0 ml · min-1.结果:栀子苷在0.016 7～0.333 2 mg·ml-1具有良好的线性关系,r=1.000 0,平均回收率为96.10%,RSD为0.96%.结论:本试验所确定的质量分析方法稳定可靠,可作为肝宁丸中栀子苷的含量测定方法.     

HPLC法测定归龙筋骨宁胶囊中士的宁含量

目的:建立归龙筋骨宁胶囊中士的宁的HPLC含量测定方法.方法:采用Thermo HTOERSIL Silica色谱柱(250mm×4.6mm,5μm),流动相为正己烷-二氯甲烷-甲醇-三乙胺(42.5:42.5:5.5:0.1),流速1.0ml/min,检测波长为254nm.结果:线性范围O.0660μg~0.6600μg(r=0.9999),呈良好线性关系,士的宁的平均加样回收率为99.38%,RSD=0.74%.结论:本方法操作简便,分离效果好,结果准确.     

HPLC法测定强筋健骨丸中马钱子碱和士的宁的含量

目的建立强筋健骨丸中马钱子碱和士的宁的含量测定方法。方法采用HPLC法,色谱柱为Ultimate XB-C_(18)(250 mm×4.6 mm,5μm);乙腈-0.01 mol·L~(-1)庚烷磺酸钠与0.02 mol·L~(-1)磷酸二氢钾等量混合溶液(用体积分数为10%的磷酸调节pH值至2.8)(21∶79)为流动相;检测波长为260 nm。结果马钱子碱和士的宁的含量分别在0.063～1.575(r_1=0.999 9)和0.075～1.875μg(r_2=0.999 9)范围内线性关系良好,回收率在98.1%～102.2%之间,RSD值均小于5.0%。结论该方法准确、稳定、可靠,可用于强筋健骨丸中马钱子碱和士的宁的质量控制。     

HPLC法测定矽肺宁片中岩白菜素的含量

目的:采用高效液相法测定矽肺宁片中岩白菜素的含量.方法:以甲醇-水(20:80)为流动相,迪马C18柱(250mm×4.6mm,5μm)为固定相,检测波长为275nm.结果:岩白菜素在0.88～7.04μg范围内呈良好的线性关系,r=0.9997,平均回收率为99.35%(n=6),RSD=0.93%.结论:本法操作简便准确,可作为矽肺宁片中岩白菜素的质量控制方法.     

RP-HPLC法测定地牡宁神口服液中马钱苷的含量

目的:建立RP-HPLC法测定地牡宁神口服液中马钱苷的含量.方法:采用SHIMADZU Shim-pack vp-ODS(250 mm×4.6 mm, 5μm)色谱柱,流动相:甲醇-水-甲酸(30:69:1),检测波长:240nm流速:1.0 ml·min-1.结果:马钱苷的线性范围为0.16～5.56μg,r=0.9998,平均回收率为101.7%(RSD=1.5%,n=5).结论:方法简便、准确,可用于地牡宁神口服液的质量控制.     

高效液相色谱法测定妇炎康丸中芍药苷的含量

目的:建立高效液相色谱法测定妇炎康丸中芍药苷的含量。方法:色谱柱为Kromasil C18(250 mm×4.6 mm,5μm;以甲醇-异丙醇-冰醋酸-水(24∶3∶3∶70)为流动相;检测波长为230 nm;流速1.0 mL.min-1;进样量10μL。结果:芍药苷在21～103μg.mL-1范围内线性关系良好,r=0.999 9,平均回收率为98.5%(RSD=0.54%)。结论:该法简便、准确,可用于妇炎康丸中芍药苷的含量测定。     

RP-HPLC法测定万氏牛黄清心丸(浓缩丸)中盐酸小檗碱的含量

目的:建立万氏牛黄清心丸(浓缩丸)的含量测定方法,有效控制该制剂的质量.方法:采用RP-HPLC法测定盐酸小檗碱的含量.以乙腈-0.05mol/L磷酸二氢钾溶液(10%氢氧化钾调pH5.0)(28:72)为流动相,Polaris C18-A(250mm×4.6mm,5μm)为色谱柱;265nm为检测波长.结果:测得线性范围0.0256～0.2304μg(r=0.9999),平均回收率为99.02%,RSD=1.61%(n=5).结论:本方法可作为该制剂的质控指标.     

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.