HPLC测定利舒康胶囊中盐酸小檗碱的含量

目的:建立利舒康胶囊中盐酸小檗碱的高效液相色谱测定方法。方法:采用HYPERSILBDS C_(18)柱(150 mm×4.6 mm,10μm);流动相:乙腈-0.1 mol·L~(-1)磷酸二氢钾-0.025 mol·L~(-1)十二烷基磺酸钠(50:25:25)。流速1.0 ml·min~(-1);检测波长为345 nm。结果:平均回收率为98.9%,RSD为0.96%,方法重现性的RSD为1.33%(n=5)。盐酸小檗碱线性范围为0.194～0.972μg(r=0.9996)。结论:本法操作简便,结果准确,可用于利舒康胶囊的质量控制。     

RP—HPLC法测定黄柏中小檗碱、巴马汀和药根碱的含量

目的:建立了用外标法对黄柏中小檗碱、巴马汀和药根碱同时定量的测定方法,考察小檗碱、巴马汀和药根碱的含量与其产地的关系。方法:高效液相色谱法,色谱柱:Kromasil-C_(18)(4.6mm×250mm,5μm),流动相:甲醇-乙腈-0.1mol·L~(-1)磷酸二氢钠(磷酸调pH为3.0)-2g·L~(-1)十二烷基硫酸钠-三乙胺(25∶25∶25∶25∶0.2),流速:1.0mL·min~(-1),检测波长:230nm,柱温:室温。结果:小檗碱、巴马汀和药根碱色谱峰面积与浓度呈良好的线性关系,线性范围分别是:盐酸小檗碱:21～495μg·mL~(-1),Y=3.144×10~6X 8.644×10~4,r=0.9999;盐酸巴马汀:2.0～40μg·mL~(-1),Y=7.570×10~5X 1.622×10~3,r=0.9999;盐酸药根碱:0.32～13μg·mL~(-1),Y=4.649×10~5X 2.161×10~3,r=0.9999。平均回收率小檗碱为98.0%,RSD为2.9%;巴马汀为97.7%,RSD为2.7%;药根碱为97.5%,RSD为2.4%。结论:本方法测定了21个不同产地的黄柏样品中小檗碱、巴马汀和药根碱含量,该方法分离度好,简便,重现性好。     

RP-HPLC法测定牛黄上清丸中盐酸小檗碱的含量

目的:建立牛黄上清丸中盐酸小檗碱的含量测定RP-HPLC方法。方法:色谱柱为Diamonsil C_(18)柱(250mm×4.6mm, 5μm),流动相为乙腈-磷酸盐缓冲液[0.05mol·L~(-1)的磷酸二氢钾溶液和0.02mol·L~(-1)庚烷磺酸钠溶液(1:1),含0.2%三乙胺,用磷酸调pH至3.0(30:70),流速:1.0 ml·min~(-1),波长:265nm,柱温:35℃。结果:盐酸小檗碱的进样量在0.20～1.02μg范围内线性关系良好(r=0.999 9),平均回收率为99.4%,RSD=1.9%(n=6)。结论:方法准确、可靠,可用于牛黄上清丸的质量控制。     

HPLC法测定玛木然止泻胶囊中盐酸小檗碱与没食子酸的含量

目的采用高效液相色谱法测定玛木然止泻胶囊中盐酸小檗碱和没食子酸的含量。方法色谱柱为Ecosil C18色谱柱(250mm×4.6mm,5μm)。盐酸小檗碱流动相为乙腈-0.05mol·L~(-1)磷酸二氢钾溶液(30∶70),检测波长为345nm,流速为1.0mL·min~(-1);没食子酸流动相为甲醇-2mL·L~(-1)磷酸溶液梯度洗脱,检测波长为270nm,流速为1.0mL·min~(-1)。结果盐酸小檗碱和没食子酸分别在0.211~2.109(r=0.999 1)及0.207~2.071μg·mL~(-1)(r=0.999 6)范围内线性关系良好;平均加样回收率分别为98.20%(RSD=2.20%)和102.52%(RSD=1.28%)。结论该方法准确、简便、重复性好,可用于玛木然止泻胶囊的质量控制。     

高效液相色谱法测定黄柏地榆胶囊中盐酸小檗碱含量

目的:建立黄柏地榆胶囊中盐酸小檗碱的高效液相色谱含量测定方法。方法:采用Shim-pack vp-ODS柱(250mm×4.6mm,5μm),以乙腈-0.05mol·L~(-1)磷酸二氢钾缓冲液(含三乙胺0.5%,磷酸调pH至3.0)(36:64)为流动相,流速为1.0ml·min~(-1),检测波长为345nm。结果:盐酸小檗碱在1.97～31.55μg·ml~(-1)范围内有良好线性关系,r=0.999 9。平均回收率98.6%,RSD为2.1%(n=6)。结论:方法简便、准确、重复性好,可用于该制剂的质量控制。     

金鸡颗粒中药材的鉴别与盐酸小檗碱的测定

目的 采用薄层鉴别法定性鉴别金鸡颗粒中的药材和采用HPLC法测定盐酸小檗碱的含量.方法 用用Diamonsil(钻石)C_(18)柱(150 mm×4.6 mm,5 μm),流动相为0.033 mol·L~(-1)磷酸二氢钾溶液-乙腈(70:30),流速1 mL·min~(-1),柱温30℃.结果 金鸡颗粒的薄层鉴别方法分离度好、专属性强、简单可行;盐酸小檗碱的线性范围为0.0196～0.1470 μg(,=0.9999),平均回收率为99.8%,RSD=0.9%.结论 所建方法适用于金鸡颗粒的质量控制.     

复方芒果苷滴眼液中芒果苷和盐酸小檗碱的鉴别及含量测定

目的 采用TLC定性鉴别复方芒果苷滴眼液中的芒果苷和盐酸小檗碱并用HPLC测定其含量.方法 用C_(18)柱,流动相为乙腈-0.05 mol·L~(-1)磷酸二氢钾缓冲液(28:72),流速1.0 mL·min~(-1),检测波长265 nm,外标法定量.结果 芒果苷和盐酸小檗碱的线性范围均为0.1～1.0 μg,平均回收率分别为101.0%(RSD=2.09%,n=9)、100.6%(RSD=1.87%,n=9).结论 所建方法简便、准确,可用于复方芒果苷滴眼液的质量控制.     

HPLC测定结肠炎散中盐酸小檗碱含量

目的:建立结肠炎散中盐酸小檗碱含量测定方法。方法:采用高效液相色谱法,用Hypersil ODS2 C_(18)色谱柱(250mm×4.6mm,5μm);流动相:乙腈-0.03mol·L~(-1)磷酸二氢钾溶液(55:45);柱温:室温;检测波长:265nm。结果:盐酸小檗碱浓度在0.04～0.2g范围内与峰面积呈良好线性关系,r=0.9996,平均回收率为100.21%(RSD为0.49%)。结论:本方法专属、重复性好,可用于结肠炎散中盐酸小檗碱的含量测定。     

RP-HPLC法测定荜铃胃痛颗粒中盐酸小檗碱的含量

本文建立测定荜铃胃痛颗粒中盐酸小檗碱含量的反相高效液相色谱法。采用DiamonsilODS—C_(18)色谱柱,流动相：乙腈—0．02mol．L~1磷酸二氢钾(25：75,用磷酸调节流动相的pH值至3．0),检测波长：347nm；流速：1．0ml·min~(-1)。盐酸小檗碱在4．16～62．42μg·ml~(-1)浓度范围内呈良好线性关系,相关系数为0．9999,平均回收率100．72%,RSD为0．9%(n=5)。本方法简便、准确、重复性好,可用于荜苓胃痛颗粒中盐酸小檗碱的含量测定。     

反相高效液相色谱法测定黄连及制剂中小檗碱的含量

目的:测定黄连及其制剂中小檗碱的含量.方法:反相高效液相色谱法,Hypersil ODS C18柱(250 mm×4.6 mm,10 μm);流动相:乙腈(含0.025 mol·L-1磷酸二氢钾与0.025 mol·L-1庚烷磺酸钠的溶液)-水相(含0.2%三乙胺,用磷酸调节pH 3.0)(40∶60);检测波长为350 nm.结果:盐酸小檗碱在4～200 mg·L-1浓度范围内,峰面积与其浓度呈良好的线性关系;片剂中盐酸小檗碱的平均回收率为100.4%,RSD为0.61%.结论:方法简便,快速,准确.可分离和测定黄连药材中各成分及其制剂小檗碱的含量.     

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.