气相色谱法测定辣椒风湿膏中薄荷脑与冰片的含量

目的建立辣椒风湿膏中薄荷脑与冰片的含量测定方法。方法采用气相色谱法,用水蒸气蒸馏法提取薄荷脑、冰片,以萘作为内标物,使用PEG20M色谱柱,用氢火焰离子检测器检测。结果通过方法学考察,薄荷脑在1.008μg～5.042μg范围内呈良好的线性关系,平均回收率为95.9%(n=5)。冰片在1.008μg～5.040μg范围内呈良好的线性关系,平均回收率为96.0%(n=5)。结论方法简便、准确、重现性好、精密度高。可用于控制辣椒风湿膏的质量。     

气相色谱法测定辣椒风湿膏中薄荷脑与冰片的含量

目的 建立辣椒风湿膏中薄荷脑与冰片的含量测定方法。方法 采用气相色谱法，用水蒸气蒸馏法提取薄荷脑、冰片，以萘作为内标物，使用PEG-20M色谱柱，用氢火焰离子检测器检测。结果 通过方法学考察，薄荷脑在1．008μg～5．042μg范围内呈良好的线性关系，平均回收率为95．9％（n=5）。冰片在1．008μg～5．040μg范围内呈良好的线性关系，平均回收率为96．0％（n=5）。结论 方法简便、准确、重现性好、精密度高。可用于控制辣椒风湿膏的质量。     

气相色谱法测定止痒消炎水中薄荷脑、冰片和麝香草酚的含量

目的建立同时测定止痒消炎水中薄荷脑、冰片和麝香草酚含量的气相色谱测定方法。方法采用气相色谱内标法,FID检测器,HP-INNDW AX石英毛细管柱(30m×250μm,0.25μm),应用程序升温(140℃保持4.1min以后20℃.min-1升至240℃),进样口温度200℃,检测器温度250℃;分流进样,分流比10:1。结果薄荷脑在0.32～3.2mg.mL-1,冰片在0.56～5.6mg.mL-1,麝香草酚在0.16～1.6mg.mL-1内呈良好的线性关系,加样回收率,薄荷脑为99.8%,(RSD=1.3%);冰片为99.2%(RSD=1.5%);麝香草酚为99.8%(RSD=0.9%)。结论该方法简单可靠,适合于止痒消炎水中薄荷脑、冰片和麝香草酚的含量测定。     

气相色谱法测定脚气水中的冰片和薄荷脑的含量

目的:用气相色谱内标法直接测定脚气水中的冰片和薄荷脑的含量.方法:采用DB-FFAP石英毛细管柱(30 m×0.32 mm×0.25 μm),程序升温:初始温度100℃以3℃·min-1升到150℃保持4 min,进样口温度200℃,检测器温度200℃;分流进样,分流比1:10.结果:薄荷脑和冰片均在0.4～1.2μg范围内呈良好的线性关系(r≥0.999).平均回收率薄荷脑为97.64%,RSD=2.3%(n=6);冰片为98.69%,RSD=2.4%(n=6).结论:该方法简单可靠,重现性好,适合于脚气水中冰片和薄荷脑的含量测定.     

狗皮膏(改进型)质量标准研究

目的:修订提高狗皮膏(改进型)的质量标准。方法:用薄层色谱法对狗皮膏(改进型)中当归进行定性鉴别;用气相色谱法对狗皮膏(改进型)中冰片、薄荷脑及水杨酸甲酯进行定性鉴别,并测定处方中冰片、薄荷脑及樟脑的含量;用高效液相色谱法测定处方中盐酸苯海拉明的含量。结果:当归的薄层色谱鉴别斑点清晰,重现性好,无干扰;龙脑在0.03~0.26μg,薄荷脑在0.07~0.71μg,樟脑在0.05~0.46μg,盐酸苯海拉明在0.56~5.59μg范围内线性关系良好,各成分平均回收率分别为99.74%(龙脑)、99.10%(薄荷脑)、99.08%(樟脑)、96.95%(盐酸苯海拉明)。结论:修订后的质量标准简便易行,可有效控制狗皮膏(改进型)的质量。     

熊胆丸的质量标准研究

目的:建立熊胆丸的质量标准。方法:采用薄层色谱(TLC)法对制剂中熊胆、黄连、龙胆、栀子进行定性鉴别;采用毛细管气相色谱法对样品中冰片、薄荷脑进行定量测定。结果:TLC斑点清晰、分离度好,阴性无干扰;冰片、薄荷脑的检测浓度分别在56.9～683.3(r=0.9987)、56.0～672.0(r=0.9984)μg.mL-1范围内与各自峰面积积分值呈良好线性关系,平均回收率分别为98.68%、99.07%,RSD分别为1.1%、1.0%(n均为9)。结论:所建标准可用于熊胆丸的质量控制。     

不同厂家三七伤药片中冰片的气相色谱法含量测定

目的:建立三七伤药片中冰片的气相色谱法含量测定方法。方法:采用气相色谱法、Agilent DB-WAXetr聚乙二醇(PEG)气相毛细管柱(30 m×250μm,0.25μm)和氢火焰离子化法测定三七伤药片中冰片的含量。结果:三七伤药片中,冰片的含量是在23.61～787.13μg/mL范围内呈现良好的线性关系,平均加样回收率为97.21%(RSD为0.87%),三七伤药片中冰片的含量为0.11～1.13 mg/片。结论:该方法准确、稳定、可靠,适用于测定三七伤药片中冰片的含量,为三七伤药片的质量控制提供参考。     

毛细管气相色谱法同时测定少林风湿跌打膏中薄荷脑、水杨酸甲酯和冰片的含量

目的:建立毛细管气相色谱法同时测定少林风湿跌打膏中薄荷脑、水杨酸甲酯和冰片的含量。方法:采用水蒸气蒸馏法提取制备样品溶液。HP-INNOWax Polyethylene Glycol(30 m×0.35 mm×0.25μm)石英毛细管色谱柱,柱温110℃,进样口温度200℃,氢火焰离子化检测器(FID),分流进样,分流比10.0∶1,载气为氮气,流速1.0 mL.min-1,进样量1μL。结果:薄荷脑在0.423~2.642 mg.mL-1范围内与峰面积呈良好线性关系(r=0.9999),水杨酸甲酯在0.405~2.532 mg.mL-1范围内与峰面积呈良好线性关系(r=0.9999),冰片在0.412~2.575 mg.mL-1范围内与峰面积呈良好线性关系(r=0.9999);平均加样回收率薄荷脑为102.2%(RSD=2.0%),水杨酸甲酯为102.1%(RSD=2.0%),冰片为102.5%,(RSD=2.0%)。结论:本方法简便、准确、重现性好,可用于少林风湿跌打膏制剂及中间体的质量控制。     

GC法测定蛇脂冰肤软膏中薄荷脑和冰片的含量

目的:采用气相色谱法测定蛇脂冰肤软膏中薄荷脑、冰片的含量。方法:样品经正己烷超声处理后,采用Agilent INNO-WAX毛细管色谱柱(30 m×0.25 mm×0.25μm);FID检测器;色谱条件:柱温:110℃,载气流速1.5 mL.min-1,进样口温度:250℃,检测器温度:300℃。进样量:1μL。结果:薄荷脑在0.0762～6.0995 mg.mL-1范围内线性关系良好(r=0.9999,n=6),龙脑在0.0460375～3.683 mg.mL-1范围内线性关系良好(r=0.9999,n=6)。薄荷脑的平均加样回收率(n=9)为101.1%,龙脑的平均加样回收率(n=9)为101.7%。结论:该方法灵敏度高、专属性好、操作简便、重现性好。     

熊胆丸定性定量方法的研究

目的:建立熊胆丸的定性定量方法。方法:采用TLC法对方中的熊胆、黄连、龙胆、栀子进行定性鉴别;采用GC法同时测定熊胆丸中冰片、薄荷脑的含量。采用安捷伦DB-WAX毛细管柱(30 m×0.45 mm×0.85μm),载气为氮气,FID检测器,流速:3.0 mL.min-1;分流比为25∶1;进样体积为1μL。结果:TLC色谱中可检出熊胆、黄连、龙胆、栀子;龙脑浓度在56.0～672.0μg.mL-1范围内呈线性关系,3个浓度的平均回收率(n=3)分别为99.4%,101.6%,100.7%;薄荷脑浓度在56.9～683.3μg.mL-1内呈线性关系,3个浓度的平均回收率(n=3)分别为101.4%,100.0%,101.3%。结论:该方法操作简便,重复性好,结果准确可靠,适用于该药的质量控制。     

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.