气相色谱法同时测定醒脑静氯化钠注射液中冰片及麝香酮的含量

建立气相色谱同时测定醒脑静氯化钠注射液中冰片及麝香酮含量.以氯仿为溶剂提取醒脑静氯化钠注射液中的冰片及麝香酮,用聚乙二醇-20M毛细管色谱柱,FID检测器,程序升温140℃维持8分钟,再以30℃·min-1升温至200℃维持10分钟,采用外标法测定.结果冰片在13.65～271.8μg·ml-1浓度范围内线性相关(r=0.9999), 回收率为98.62%,RSD=1.80% ,(n=6);麝香酮在2～40μg·ml-1浓度范围内线性相关(r=0.9999),回收率为97.80%,RSD=1.37% ,(n=6). 该方法准确,灵敏,重现性好.     

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.     

气相色谱法测定醒脑静注射液中麝香酮含量

目的建立气相色谱法测定醒脑静注射液中麝香酮的含量。方法采用气相色谱法,色谱柱为DB-1毛细管柱15m×0.53mm×1μm,FID检测器,采用外标法测定。结果用气相色谱法测定醒脑静注射液中麝香酮在8.706~174.12μg.mL-1范围内呈线性关系,线性方程为Y=19.3951＋4.1671X,相关系数r=0.9993（n=5）,平均回收率为100.5%,RSD1.31%（n=9）。结论本方法简便、准确、快速,可用于醒脑静注射液的质量控制。     

固相萃取-手性气相色谱法测定醒脑静注射液中右旋龙脑和麝香酮的含量

目的 建立固相萃取-手性气相色谱测定醒脑静注射液中右旋龙脑和麝香酮含量的方法.方法 醒脑静注射液直接经C18固相萃取柱前处理,用无水乙醇洗脱,洗脱液以手性气相色谱柱测定右旋龙脑和麝香酮的含量.毛细管色谱柱为CYCLOSIL-B(30m×0.25 mm×0.25μm),进样口为200℃,FID检测器为220℃,采用程序升温118℃保持2min,以50℃/min升至220℃保持10min.结果 右旋龙脑的平均回收率为100.4％,RSD =0.9％ (n =6),线性范围0.048mg· mL-1 ～0.57mg·mL-1,r=0.9999;麝香酮的平均回收率为96.5％,RSD =0.9％ (n =6),线性范围2.31μg· mL-1～23.2μg· mL-1,r =0.9999.结论 该方法前处理非常简便,结果准确可靠,可用于醒脑静注射液的质量控制.     

毛细管气相色谱法测定醒脑静葡萄糖注射液中冰片和麝香酮含量

目的建立醒脑静葡萄糖注射液中冰片和麝香酮的含量测定方法。方法使用气相色谱仪,采用DM-17毛细管色谱柱（50％苯基和50％甲基聚硅氧烷）,0.32mm×30m,液膜厚度为0.25μm;柱温70℃,保持2min,以10℃·min^-1的速度升温至200℃,保持10min。以氮气为载气,流速为2ml·min^-1;FID检测器。结果冰片,麝香酮线性关系良好,相关系数均大于0.999;平均回收率分别为97.2％、97.0％;检出限分别为0.25、0.16mg·L^-1。结论本方法简便,灵敏度高,重复性好,结果准确,适合于醒脑静葡萄糖注射液中冰片和麝香酮的含量测定。     

气相色谱法拆分醒脑静注射液中龙脑对映体及含量测定

目的:采用气相色谱法拆分醒脑静注射液中龙脑对映体,并通过对映体的分离测定含量。方法:采用CYCLOSIL-B(30m×0.25 mm×0.25μm)手性毛细管色谱柱、FID检测器,以内标法测定醒脑静注射液中左旋龙脑和右旋龙脑的含量。结果:龙脑对映体在CYCLOSIL-B手性毛细管色谱柱上具有较好的分离效果,其分离度为2.04。左旋龙脑和右旋龙脑线性范围分别为0.048～0.960和0.050～1.008 mg·mL-1(r≥0.9991);冰片投料为天然冰片的样品中右旋龙脑平均回收率(n=6)为98.4%,RSD为1.8%;冰片投料为艾片的样品中左旋龙脑的平均回收率(n=6)为99.1%,RSD为1.9%。结论:所建立的方法简单、准确、可靠,能用于醒脑静注射液的质量控制。     

心灵丸质量控制方法研究

目的:建立心灵丸的质量标准.方法:采用薄层色谱(TLC)法鉴别处方中冰片、人参、三七、人工麝香、人工牛黄;用高效液相色谱(HPLC)法测定心灵丸中蟾酥(华蟾酥毒基和脂蟾毒配基)的含量.色谱柱为Hypersil ODS2(5μm,4.6mm×200 mm),流动相为乙腈-0.5%磷酸二氢钾溶液(用磷酸调节pH至3.2)(45:55),检测波长为296 mm,柱温30℃.结果:华蟾酥毒基在0.9～22.5 rng·L-1的范围内,脂蟾毒配基在0.9～22.2 nag·L-1的范围内呈良好线性关系,心灵丸中华蟾酥毒基平均回收率为99.79%(RSD=1.6%,n=9),脂蟾毒配基平均回收率为100.32%(RSD=1.7%,n=9).结论:所建立的TLC和HPLC方法专属性强,重复性好,可用于心灵丸的质量控制.     

GC测定苍耳子鼻炎胶囊中薄荷脑和冰片含量

目的 建立苍耳子鼻炎胶囊中薄荷脑和冰片的含量测定方法.方法 采用聚乙二醇(PEG)-20M填充柱(涂布浓度为10%);柱温:150℃;进样口温度:210℃;FID检测器,检测器温度:230℃.结果 薄荷脑线性范围为0.395～3.162μg(r=0.9999),平均回收率为100.38%,RSD为0.94%(n=9);冰片线性范围为0.386～3.088μg(r=0.9998),平均回收率为99.43%,RSD为1.0%(n=9).结论 本法灵敏、准确,重现性好,可以用于测定苍耳子鼻炎胶囊中薄荷脑和冰片的含量.     

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。     

醒脑再造丸质量标准研究

目的：建立醒脑再造丸（黄连、冰片、木香等）的质量标准。方法：采用TLC法鉴别处方中的黄连、冰片和木香;用HPLC—ELSD法测定黄芪中黄芪甲苷的含量,色谱柱PhenomenexGeminiC18（4．6mm×250mm,5μm）,流动相：乙腈-水（36：64）;流速为1．0mL·min^-1;漂移管温度为105℃;载气流速：2．7L·min^-1。结果：TLC法鉴别色谱特征斑点明显,黄芪甲苷在0．486～2．43μg范围内呈线性关系,r=0．9997;平均回收率为101．7％（n=6）,RSD=0．5％。结论：所建立的TLC和HPLC-ELSD方法操作简便,结果准确,重复性好,可用于醒脑再造丸的质量控制。     

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.