高效液相色谱法测定扑米酮中的杂质苯巴比妥含量

采用高效液相色谱法测定扑米酮中特殊杂质苯巴比妥的含量。色谱柱μ-Bondsphere C_(18)(3.9mm×150mm,5μm)流动相为甲醇-水(18:32),检测波长254nm。线性范围为0.05～0.3μg(n=5,r=0.9998),平均回收率为100.2％(n=5,RSD=1.737％)。     

高效液相色谱法测定扑米酮中的杂质苯巴比妥含量

采用高效液相色谱法测定扑米酮中特殊杂质苯巴比妥的含量。色谱柱μ-Bondsphere C₁₈(3.9mm×150mm,5μm)流动相为甲醇-水(18:32),检测波长254nm。线性范围为0.05～0.3μg(n=5,r=0.9998),平均回收率为100.2％(n=5,RSD=1.737％)。     

气相色谱法测定然降多吉胶囊中麝香酮的含量

目的:建立用气相色谱法测定然降多吉胶囊中麝香酮含量的方法.方法:样品用无水乙醇提取,采用DB-1色语柱(30 m×0.32 mm,l.00 μm),氮火焰离子化检测器(FID),柱温为初始温度150℃,以每分钟5℃的速率升温至230℃,保持10 min,分流进样,分流比为5:1.结果:麝香酮在0.029136 μg～7.284 μg范围内与峰面积的线性关系良好(r=0.99985);测得平均回收率(n=6)为 100.10%,RSD为1.10%.结论:本方法灵敏度高、重现性好,结果准确可靠.     

GC同时测定麝香通心滴丸中龙脑、异龙脑和麝香酮的含量

摘要：目的 建立同时测定麝香通心滴丸中龙脑、异龙脑及麝香酮含量的气相色谱法。方法 色谱柱：HP-5MS毛细管色谱柱(30 m×0.32 mm,0.25 μm),检测器为FID检测器,检测器温度为250 ℃,进样口温度220 ℃。柱温以100 ℃为初始温度,保持2分钟,以2 ℃?min-1升温至110 ℃,保持3分钟,以50 ℃?min-1升温至205 ℃,保持7分钟,以20 ℃?min-1升温至250 ℃,保持2分钟;载气为氮气,流速为1 mL?min-1;进样方式为分流进样,分流比为10：1;进样量为1 μL,以萘为内标。结果 龙脑、异龙脑、麝香酮的浓度分别在0.05468~0.4374 mg?mL-1(r=0.9999),0.07067~0.5654 mg?mL-1(r=0.9999),0.004512~0.03610 mg?mL-1(r=0.9997)的范围内线性良好;平均回收率分别为97.91 %(RSD=2.05 %),100.79 %(RSD= 2.78 %),105.36 %(RSD=3.78 %)。结论 该方法有效可靠,可用于麝香通心滴丸中龙脑、异龙脑和麝香酮的含量测定。     

HPLC-ELSD测定硫酸西索米星注射液中的主药

目的 建立测定硫酸西索米星含量的方法.方法 采用HPLC-ELSD法,色谱柱为Waters SunFire C18柱(150 mm×4.6 mm,5 μm),流动相为1.5%三氟醋酸-甲醇(95:5),流速为1.0 ml·min-1,柱温为30℃,漂移管温度为60℃,雾化气体压力为25 psi.结果 回归方程为:Y=1.235X+6.156,线性范围为1.0～10.0 μg(r=0.99998);回收率为98.9%(n=9),RSD=0.86%.结论 所建方法操作简便、准确、重复性好,可用于硫酸西索米星注射液的含量测定.     

气相色谱法测定六神丸中麝香酮含量

目的建立测定六神丸中麝香酮含量的气相色谱法。方法样品用乙酸乙酯浸渍提取后进样,采用HP50＋石英毛细管色谱柱（30m×0.53mm,1μm）,以N2为载气,柱温165℃,进样口温度150℃,火焰离子化检测器温度190℃。结果麝香酮质量浓度在23.90～1195.00μg/mL范围内与峰面积线性关系良好（r=0.9997）,麝香酮的平均回收率为99.16%,RSD为1.04%（n=9）。结论气相色谱法简单、准确,可用于六神丸的质量控制。     

毛细管气相色谱法测定莪术油中吉玛酮和β-榄香烯的含量

目的建立以毛细管气相色谱法测定莪术油中吉玛酮和β榄香烯含量的方法。方法内标法,以水杨酸甲酯为内标物。采用OV 1701为固定液,柱长25 m、内径0.2 mm、液膜厚度0.25μm的毛细管色谱柱;程序升温:起始温度100℃,5℃.min-1,结束温度200℃;载气为氮气,流速1.5 mL.min-1。氢火焰离子化检测器。结果吉玛酮进样量在0.077~0.384μg内与峰面积比值(吉玛酮/水杨酸甲酯)呈良好的线性关系,r=0.999 8(n=5),平均回收率99.1%(RSD 0.85%,n=6);β榄香烯进样量在0.715~14.300 ng内与峰面积比值(β榄香烯/水杨酸甲酯)呈良好的线性关系,r=0.999 9(n=5),平均回收率100.4%(RSD 0.58%,n=6)。结论毛细管气相色谱法可作为莪术油中吉玛酮和β榄香烯的含量测定方法。     

毛细管气相色谱法测定理中气雾剂中龙脑的含量

目的建立毛细管气相色谱法测定理中气雾剂中龙脑的含量.方法使用聚乙二醇(PEG)-20M毛细管色谱柱(30 m×0.32 mm,0.25 μm);以萘为内标,分流进样,分流比为101;柱温为100 ℃;进样口温度210 ℃,检测器温度220℃;栽气为氮气;流速为4.5 mL·min-1.结果龙脑在0.113～0.906 μg范围内线性关系良好,r=0.999 7,平均加样回收率为101.6%,RSD为1.33%.结论该方法简便,重复性好,可用于理中气雾剂中龙脑的含量测定.     

气相色谱法测定无极膏中5种成分的含量

目的建立一种用气相色谱法测定无极膏中5种成分含量的方法.方法采用HP-INNOWAX Polyethylene Glycol(30.0 m×250 μm×0.25 μm)毛细管色谱柱,柱温采用程序升温,进样口温度200℃,FID检测器,检测器温度250℃.结果样品中5种成分完全分离且线性关系良好,樟脑、薄荷脑、龙脑、水杨酸甲酯、麝香草酚的加样回收率分别为97.3%、98.9%、98.3%、101.3%和100.8%(n=9).结论该法简便快速,结果准确,可以有效地控制质量.     

气相色谱法测定伤科止痛膏中麝香酮的含量

目的:建立伤科止痛膏中麝香酮的含量测定方法.方法:色谱柱为HP-INNOWAX 30 m×0.53 mm,1.Oμm film,FID检测器,采用程序升温,进样口温度:250℃;检测器温度:250℃.结果:麝香酮浓度在5.6688 μg·mL(-1)-226.752 μg·mL(-1)范围内线性关系良好,相关系数r=0.9997.,加样回收率为99.96%,RSD为1.38%.结论:方法准确、灵敏、重现性好,可用于伤科止痛膏的质量控制.     

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.     

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.     

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.     

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.