紫苏叶油中紫苏酮的含量测定

目的建立紫苏叶油中紫苏酮的含量测定方法。方法采用气相色谱法,色谱条件:色谱柱为DB-17石英毛细管柱(30 m×0.25 mm,0.25μm);进样口温度280℃;分流比为50∶1;检测器温度为280℃;进样量1μL;程序升温:初始温度100℃,保持5 min,以每分钟5℃的速率升温至120℃,保持2 min,再以每分钟10℃的速率升温至230℃,保持1 min。结果紫苏酮进样量在0.2～1.6μg与峰面积积分值呈良好的线性关系(r=0.999 9);平均加样回收率为100.7%,RSD为0.43%(n=6)。结论采用气相色谱法对紫苏叶油中紫苏酮进行测定,方法简便,快速、准确,重复性好。     

顶空气相色谱法测定醋酸奥曲肽原料中的残留溶剂

目的：采用顶空气相色谱法测定醋酸奥曲肽原料中的残留溶剂。方法：采用6%腈丙基苯基-94%二甲基聚硅氧烷(DB-624)毛细管色谱柱(30 m×0.32 mm×0.25 μm),柱温为程序升温：初始温度为40 ℃,保持4 min,然后以20 ℃?min-1的升温速率升至200 ℃,保持15 min,进样口温度200 ℃,氢火焰离子化检测器,检测器温度280 ℃,分流比2:1,载气流速为1.0 mL?min-1。结果：4种残留溶剂均能完全分离,甲醇、乙腈、二氯甲烷、N,N-二甲基甲酰胺线性范围分别为19.89～318.18mg?mL-1 (r=0.999 7)、4.19～67.07mg?mL-1 (r=0.999 7)、11.69～58.44mg?mL-1 (r=0.999 7)和20.38～122.28mg?mL-1 (r=0.999 7);检测限分别为1.30、0.03、0.02μg和3.76μg。结论：该方法重复性好,灵敏度高,可用于醋酸奥曲肽原料中的残留溶剂控制。     

气相色谱法测定保济丸中百秋李醇的含量

目的:建立以气相色谱法测定保济丸中百秋李醇含量的方法,制定并完善保济丸的质量标准。方法:采用非极性毛细管柱AT.SE-54(15m×0.25mm×0.33μm),柱温采用程序升温:起始150℃,保持23min,以8℃·min-1速率升至230℃,保持2min,进样口温度为280℃,检测器(FID)温度为280℃,载气为氮气,流速为1.0mL·min-1。结果:百秋李醇进样量在0.12～0.36μg范围内线性关系良好(r=0.9999),平均加样回收率为98.62%,RSD=4.69%。结论:该方法稳定、结果可靠、重复性好,可作为保济丸质量控制标准之一。     

毛细管顶空进样法测定更昔洛韦中有机溶剂残留量

目的建立以正丁醇为内标物,测定更昔洛韦中甲醇、乙醇、丙酮和甲苯殘留量的顶空气相色谱法。方法用AgilentHP5毛细管柱(30m×0.32mm×0.25μm);载气为N2,柱流量为0.8mL/min,分流比为5:1,柱温为50℃;检测器为FID,检测器温度为250℃;Agilent7694E顶空进样器,顶空瓶加热温度为90℃,加热30min;进样口温度为200℃。结果甲醇、乙醇、丙酮和甲苯的线性范围分别为:20.23～202.3μg/mL(r=0.9995),30.05～300.5μg/mL(r=0.9992),29.82～298.2μg/mL(r=0.9993)和5.05～50.5μg/mL(r=0.9996);最低检出浓度分别为:1.95,2.52,0.18和0.12μg/mL;平均回收率分别为97.22%(RSD=2.13%),96.35%(RSD=1.65%),101.2%(RSD=3.02%)和95.45%(RSD=1.05%)。结论本法简便、灵敏、准确,适用于更昔洛韦中有机溶剂殘留量的测定。     

氯雷他定原料药中残留溶剂检测方法的研究

建立氯雷他定原料药中有机溶剂残留量测定方法。以Agilent FFAP弹性石英毛细管柱(聚乙二醇为固定液,50 m×320μm×0.5μm)为色谱柱,进样口温度为220℃;氢火焰离子化检测器(FID)温度为240℃;柱温为程序升温,初始温度40℃,保持10 min,以20℃.min-1升温至200℃,保持3 min;载气为氮气,流速3 mL.min-1。此色谱条件下被测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度良好,可用于氯雷他定原料药中有机溶剂残留量检测。     

气相色谱法测定医用棉签中环氧乙烷残留量

目的建立医用棉签中环氧乙烷残留量的测定方法。方法以水为溶剂,DM-624(6%氰丙苯基-94%二甲基聚氧硅烷)石英毛细管柱(30m×0.53mm,3.0μm),FID检测器,以高纯氮为载气,进样口温度200℃,检测温度250℃,对柱温采用程序升温法(35℃保持5min,以30℃/min升至150℃,保持5min),柱前压40kPa,采用顶空进样法进样,顶空温度60℃加热30min,进样量1mL。结果样品中环氧乙烷能与相邻杂质良好分离,浓度与峰面积的线性范围为0.2715～2.7150μg/mL(r=0.999),回收率为96.5%(RSD=2.0%),检出限为0.3mg/kg。结论气相色谱法操作简单、快捷,可以用于医用棉签中环氧乙烷残留量的控制。     

气相色谱法测定西黄胶囊中麝香酮的含量

目的建立测定西黄胶囊中麝香酮的气相色谱法。方法色谱柱:OV-17毛细管柱(30.0m×0.32mm,1.0μm);初始柱温:150℃,保持26min;再以20℃.min-1的升温速率升至230℃,保持20min;进样口温度:200℃;检测器温度:250℃;载气:氮气;流速:2.0mL.min-1。结果回归方程线性关系良好,线性范围为1.5～299.2mg.L-1,平均回收率为94.7%,RSD1.3%。结论该方法准确、灵敏,能有效控制西黄胶囊的质量。     

气相色谱法测定聚山梨酯80中二甘醇的含量

目的建立一种气相色谱法测定聚山梨酯80中二甘醇的含量.方法色谱柱:以聚乙二醇(PEG-20M)为固定液的极性毛细管柱(30m×0.32mm,0.50μm);检测器:氢火焰离子检测器(FID);检测器温度230℃;进样口温度200℃;柱温度:程序升温,初始温度60℃,保持3min,再以10℃·min-1升温至230℃保持10min;载气:高纯氮气.结果二甘醇线性范围为0.025～0.25mg·mL-1(r=0.9993);平均回收率101.57%(RSD=1.505%,n=5).结论本方法简单、结果准确、重现性好,可用于聚山梨酯80中二甘醇含量的测定.     

GC法测定香茅中香叶醇的含量

目的:建立测定香茅中香叶醇含量的方法。方法:采用超声提取法提取香茅中香叶醇,通过气相色谱法测定香叶醇的含量。色谱柱为Agilent Technologies DB-WAX(30m×0.25mm×0.25μm),以聚乙二醇(PEG-20M)为固定相,柱温为130℃,进样口温度为230℃,检测器温度为250℃,氮气(载气)流量为1.0mL.min-1,氢气(燃气)流量为40mL.min-1,空气(助燃气)流量为400mL.min-1。结果:香叶醇进样量在0.0153～0.1071μg范围内与峰面积积分值呈良好线性关系(r=0.9973);平均加样回收率为97.8%,RSD=1.68%(n=6)。结论:本方法简便、快速、准确、重复性好,可用于香茅的质量控制。     

气相色谱法测定清宣止咳颗粒中薄荷脑的含量

目的:建立测定清宣止咳颗粒中薄荷脑含量的气相色谱法。方法:采用DB-FFAP弹性石英毛细管柱(25 m×0.32 mm×0.50μm);FID检测器;载气：N₂;流速1 mL/min,进样口温度200℃,检测器温度250℃;柱温：初始温度70℃,保持4 min,然后以10℃/min升温至120℃,保持5 min,再以5℃/min升温至180℃,保持2 min,最后以25℃/min升温至200℃,保持5 min;进样量1μL;分流比2∶1。结果:薄荷脑质量浓度在0.01～0.10 mg/mL范围内与峰面积呈良好线性关系(r=0.998 5),平均回收率为99.9%(n=9,RSD=3.8%)。结论:本方法快速、简便,结果可靠、准确,重现性好,适用于清宣止咳颗粒中薄荷脑含量的测定。     

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.     

Pharmacological treatment of COVID-19: an opinion paper

The precocity and efficacy of the vaccines developed so far against COVID-19 has been the most significant and saving advance against the pandemic. The development of vaccines has not prevented, during the whole period of the pandemic, the constant search for therapeutic medicines, both among existing drugs with different indications and in the development of new drugs. The Scientific Committee of the COVID-19 of the Illustrious College of Physicians of Madrid wanted to offer an early, simplified and critical approach to these new drugs, to new developments in immunotherapy and to what has been learned from the immune response modulators already known and which have proven effective against the virus, in order to help understand the current situation.     

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.