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。     

麝香风湿跌打膏质量标准研究

目的：建立麝香风湿跌打膏的质量标准。方法：采用薄层色谱法鉴别麝香风湿跌打膏中的川芎;采用气相色谱法测定制剂中龙脑和薄荷脑的含量。结果：薄层色谱法鉴别色谱特征斑点清晰;气相色谱法测得龙脑在0.09906~0.99062 mg／ ml 范围内线性关系良好（r =0.9999,n =6）,平均回收率为101.9%,RSD 为1.9%;薄荷脑在0.14104~1.41040 mg／ ml 范围内线性关系良好（r =0.9999,n =6）,平均回收率为103.2%,RSD 为1.3%。结论：该方法快速简便,准确可靠,专属性强,重复性好,可用于麝香风湿跌打膏的质量控制。     

GC法同时测定麝香跌打风湿膏中的3种挥发性成分

目的 采用顶空气相色谱法同时测定麝香跌打风湿膏中3种挥发性成分的含量.方法 用氯仿超声溶解麝香跌打风湿膏后,以水为顶空溶剂,在80℃下平衡40 min,采用TM-WAX(50 m×0.53 mm,0.5 μm)毛细管柱、FID检测器进行气相色谱检测,程序升温,初始温度100℃,以4℃·min-1升至150 ℃,保持2 min,进样口温度200℃,检测器温度210℃.结果 樟脑、薄荷脑、水杨酸甲酯分别在10.0～160、5.17 ～82.7、7.42 ～119 μg·mL-1时线性关系良好(r樟脑=0.9994,r薄荷脑=0.9992,r水杨酸甲酯=0.9993),3者的平均回收率均在93.3％ ～101％,RSD均小于3.6％.结论 所用方法简单、快速、灵敏度高,适用于同时测定麝香跌打风湿膏中挥发性成分樟脑、薄荷脑、水杨酸甲酯的含量.     

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。     

HPLC法测定少林风湿跌打膏中大黄素和大黄酚的含量

目的：为了确保少林风湿跌打膏质量,对少林风湿跌打膏的质量进行了新的研究。方法采用高效液相色谱法（ HPLC）测定少林风湿跌打膏中大黄素和大黄酚的含量。结果大黄中的大黄素在4.25～400.25μg范围内线性关系良好,r＝0.9999,平均回收率99.78％,RSD ＝1.46％;大黄酚在7.06～706.00μg范围内线性关系良好,r＝1.0000,平均回收率99.87％,RSD ＝1.15％。结论实验方法专属性强、重复性好,准确简便。可有效的控制少林风湿跌打膏的质量。     

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。     

气相色谱法同时检测附桂风湿膏中薄荷脑、冰片和水杨酸甲酯的含量

目的建立附桂风湿膏中薄荷脑、冰片、水杨酸甲酯的GC检测方法。方法采用毛细管气相色谱法,色谱柱为EC-WAX毛细管柱(30 m×0.53 mm×0.15μm);柱温(程序升温):初始温度为80℃,保持5 min,10℃·min-1,升至180℃后保持10 min,进样口温度为180℃,检测器温度为230℃;载气为氮气,分流比为10:1,流量:7.5 mL·min-1。结果本法线性关系良好,各精密度RSD均<1.2%,薄荷脑、冰片、水杨酸甲酯的平均加样回收率分别为99.1%、98.8%、101.6%,RSD分别为2.2%、2.9%、2.1%。结论该方法操作简便快速,灵敏度高,准确度好,可作为附桂风湿膏质量控制方法。     

手性毛细管柱气相色谱法测定复方牛黄消炎胶囊中冰片的含量

目的 建立手性毛细管柱气相色谱法同时测定复方牛黄消炎胶囊中异龙脑、左旋龙脑、右旋龙脑3个成分的含量.方法 采用CYCLO-SIL-B手性毛细管柱(30m×0.25mm,0.25μm),程序升温(初始温度120℃,保持12min,以20℃/min升温至最终温度200℃,保持5min),FID检测器温度220℃,进样口温度200℃,载气为高纯N2,进样量1.0μL,进样分流比5:1.结果 异龙脑、左旋龙脑、右旋龙脑质量浓度分别在3.000~150.0μg·mL-1(r=0.9999)、1.602~80.10μg·mL-1(r=1.0000)、3.143~157.2μg·mL-1(r=1.0000)范围内与峰面积线性关系良好;平均回收率(n=6)分别为99.3%(RSD=1.8%),102.6%(RSD=2.0%),96.2%(RSD=1.9%);不同厂家复方牛黄消炎胶囊中异龙脑、左旋龙脑、右旋龙脑3个主要成分的含量范围分别为2.18~5.38、2.39~3.47、1.64~5.48mg·g-1.结论 该方法 快速、准确,精密度良好,可用于复方牛黄消炎胶囊中冰片的含量测定.     

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.     

GC法同时测定跌打镇痛膏中樟脑、薄荷脑和水杨酸甲酯含量

摘要：目的:建立同时测定跌打镇痛膏中樟脑、薄荷脑和水杨酸甲酯含量的方法。方法:样品经水蒸气蒸馏法提取后,采用气相色谱法,以奈为内标物,色谱柱:Agilent DB-WAX毛细管柱（30 m×0.32 mm,0.5μm）,进样口温度:200℃,FID检测器温度:250℃,柱温:130℃,进样量:1μl,分流比:5∶1。结果:樟脑、薄荷脑和水杨酸甲酯的分离度和线性关系良好,线性范围分别为0.409 0～4.089 6 mg·ml-1（r=0.999 9）、0.041 9～0.419 2 mg·ml-1（r=0.999 8）和0.113 8～1.138 0 mg·ml-1（r=0.999 9）;平均加样回收率分别为97.4%（RSD=0.9%）,96.8%（RSD=1.6%）和98.9%（RSD=1.2%）（n=6）。结论:该方法准确可靠,重复性好,可用于跌打镇痛膏的质量控制。     

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.     

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.