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。     

气相色谱法同时测定无极膏中5个挥发性有效成分的含量

目的:建立同时测定无极膏中合成樟脑、薄荷脑、水杨酸甲酯、冰片和麝香草酚5种主要成分含量的分析方法。方法:采用气相色谱法,色谱柱为聚乙二醇(PEG)-20M毛细管色谱柱(30 m×0.32 mm×0.25μm),检测器为FID检测器,进样口温度为250℃,检测器温度为250℃。升温程序为初始温度150℃,保持5 min;10℃.min-1升温至200℃,保持8 min;再以20℃.min-1升温至240℃,保持25 min,分流比为10∶1。结果:合成樟脑、薄荷脑、水杨酸甲酯、冰片和麝香草酚浓度分别在1.4934～7.4672 mg.mL-1(r=0.9999),0.9304～4.6520 mg.mL-1(r=0.9999),0.9075～4.5376 mg.mL-1(r=0.9999),0.1387～0.6936 mg.mL-1(r=0.9999),0.0716～0.3580 mg.mL-1(r=0.9999)质量浓度范围内线性关系良好。平均回收率(n=9)分别为98.8%,99.4%,98.6%,99.6%,99.7%。结论:该方法灵敏、快速简便、准确,可有效地控制无极膏的质量。     

气相色谱法测定复方麝香注射液中薄荷脑、龙脑含量

目的 建立气相色谱法测定复方麝香注射液中薄荷脑、冰片(以龙脑计)的含量.方法 采用气相色谱法,色谱柱为聚乙二醇-20M毛细管柱30m×0.53mm×0.25μm,程序升温,起始温度90℃,每分钟升10℃,升至170℃后保持10min,分流比50∶1,FID检测器;检测器温度为250℃.结果 用气相色谱法测定复方麝香注射液中薄荷脑在0.0871～0.5226mg·mL-1;冰片(以龙脑计)龙脑在0.1094～0.6564mg·mL-1范围内呈线性关系,线性方程分别为Y=8.7568×10-3+ 7.4529X,r=0.9999(n=5);Y=1.5603×10-2+ 7.4845X,r=0.9999(n=5),平均回收率分别为99.93％(n=9),RSD 0.8％;99.10％(n=9),RSD 1.5％.结论 本方法简便、准确、快速,可用于复方麝香注射液的质量控制.     

GC法测定痛肿灵酊中樟脑、薄荷脑、异龙脑、龙脑的含量

目的:建立气相色谱法测定痛肿灵酊中樟脑、薄荷脑、异龙脑、龙脑含量的方法.方法:色谱柱:Phenomenex ZB-WAX 石英毛细管柱(30 m×0.32 mm,0.25μm),火焰离子化检测器温度:280℃,进样口温度:250℃,柱温:130℃.结果:樟脑在0.110～5.492 μg范围内线性关系良好(r=0.999 5),平均回收率为99.04％,RSD=0.28％(n=9);薄荷脑在0.120 ～6.024 μg范围内线性关系良好(r =0.9996),平均回收率为99.16％,RSD =0.50％ (n =9);异龙脑在0.028 ～1.402 μg范围内线性关系良好(r =0.9991),平均回收率为99.03％,RSD =0.40％ (n =9),龙脑在0.034 ～ 1.700 μg范围内线性关系良好(r=0.9998),平均回收率为99.27％,RSD =0.41％ (n =9).阴性样品无干扰.结论:该法操作简便,结果准确可靠,可作为痛肿灵酊的质量控制方法.     

气相色谱法同时测定祛伤消肿酊中樟脑、薄荷脑、龙脑的含量

目的 建立祛伤消肿酊中同时测定樟脑、薄荷脑及龙脑含量的方法.方法 采用气相色谱法,FID检测器.色谱柱:HP- INNOWAX(30m×0.32mm×0.25μm);柱温:130℃;进样口温度:250℃;检测器温度:300℃.结果 樟脑、龙脑、薄荷脑回归方程的相关系数均在0.999以上,平均回收率(n=6)分别为97....     

GC法同时测定明目上清片中4个成分的含量

目的:建立同时分析测定明目上清片中4个活性成分(柠檬烯、薄荷酮、薄荷脑和胡薄荷酮)的方法。方法:采用GC法,色谱柱为DB-1701毛细管色谱柱(30 m×0.3 mm,0.25μm),柱温采用程序升温(80℃保持1 min,5℃.min-1上升至120℃,保持1 min,再以50℃.min-1的速率升温至220℃,保持2 min);进样口温度:180℃;检测器:FID;检测器温度:250℃。结果:柠檬烯、薄荷酮、薄荷脑和胡薄荷酮线性范围分别为0.0103～0.507 mg·mL-1(r=0.9997)、0.0105～0.501 mg·mL-1(r=0.9999)、0.0082～0.412 mg·mL-1(r=0.9991)、0.0085～0.404 mg·mL-1(r=0.9998);平均加样回收率(n=6)分别为99.1%、97.6%、98.7%、98.3%,RSD分别为1.2%、1.8%、1.4%、1.5%。结论:该方法可用于明目上清片的质量检测。     

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。     

GC法测定清眩片中薄荷脑的含量

目的：建立测定清眩片中薄荷脑含量的气相色谱方法。方法运用气相色谱法,采用DB-WAX毛细管柱（30 m ×0.32 mm,0.25μm）;FID检测器;柱温为110℃;分流进样,分流比为50：1。结果薄荷脑在0.04～1.00 mg＆#183; mL-1范围内与色谱峰面积呈良好的线性关系（r=0.9994）,平均回收率为99.44％,RSD为1.2％（n=6）。结论该方法简便、准确、重复性好,可用于清眩片的质量控制。     

毛细管气相色谱法同时测定沉香化气丸中3个成分的含量

目的:建立以毛细管气相色谱同时测定沉香化气丸中乙酸龙脑酯、百秋李醇、去氢木香内酯含量的方法。方法:采用SE-30(30.0 m×0.25 mm×0.25μm)色谱柱;以正十二烷为内标;柱温采用程序升温:起始温度120℃,保持5 min,以10℃.min-1升温至160℃,保持5 min,再以10℃.min-1升温至240℃,保持5 min;气化温度:260℃;检测器温度:280℃;载气为氮气,流速为3.0 mL.min-1;进样量为1μL,分流比为30∶1。结果:在选定的条件下,乙酸龙脑酯、百秋李醇、去氢木香内酯浓度分别在0.029～1.164 mg.mL-1(r=0.9999)、0.045～1.613 mg.mL-1(r=0.9999)、0.037～1.339 mg.mL-1(r=0.9995)范围内,各成分浓度与内标浓度的比值与其相应的峰面积比值呈良好的线性;平均回收率(n=9)分别为99.7%,99.5%,99.3%。结论:该方法简便准确,重复性好,可用于同时测定沉香化气丸中乙酸龙脑酯、百秋李醇、去氢木香内酯的含量。     

毛细管GC法同时测定艾叶中石竹烯与龙脑的含量

目的:建立同时测定艾叶中石竹烯与龙脑含量的方法。方法:采用毛细管气相色谱法。色谱柱为HP-5MS石英毛细管(30m×0.25mm×0.25μm),检测器为火焰离子化检测器(FID),程序升温,进样口温度为250℃,检测器温度为260℃,载气为氮气,流量为1.2mL·min-1,分流比为1∶10,内标为萘。结果:龙脑和石竹烯的进样浓度分别在0.02525～0.40400、0.04850～0.77600mg·mL-1范围内与各自峰面积积分值呈良好线性关系(r均为0.9999);平均加样回收率分别为99.20%、99.45%,RSD分别为1.82%、2.47%(n均为6)。结论:本方法简便、快速、准确,可为艾叶挥发油及其制剂的质量控制提供参考。     

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.