气相色谱法测定异丙基安替比林中的残留溶剂

目的:采用顶空进样气相色谱法测定异丙基安替比林中残留甲醇、乙醇、丙酮的残留量。方法:使用配置顶空进样器的气相色谱仪,选择固定相为6％氰丙基苯基-94％二甲基聚硅氧烷、膜厚为3．0μm,0．53mm ×30m的色谱柱,以氮气为载气,顶空进样FID检测,通过外标法计算残留溶剂的含量。结果:异丙基安替比林中有乙醇检出。乙醇的线性范围:0．10-164．96μg／mL(r=0．999 9),甲醇的线性范围:0．21-164．72μg／ mL(r=0．999 9),丙酮的线性范围:0．10-163．36μg／mL(r=1．000 0);定量限乙醇、甲醇均为0．3μg／mL,丙酮为0．1μg／mL;平均回收率甲醇为101．0％(RSD=4．8％,n=6),乙醇为99．89％(RSD=4．4％,n=6),丙酮为99．85％(RSD=3．4％,n=6)。结论:本方法简便、灵敏度高、重复性好,结果准确,可用于异丙基安替比林原料药中有机溶剂残留量的测定。     

GC法测定复方溴丙胺太林铝镁片中的薄荷脑

目的采用GC法测定复方溴丙胺太林铝镁片中薄荷脑的含量。方法采用改性聚乙二醇HP-INNOWax PolyethyleneGlycol毛细管柱(30 m×0.32 mm,0.25μm),FID检测器,载气为氮气,130℃恒温,分流比10∶1。结果薄荷脑0.19～1.91μg进样量与峰面积的线性关系良好(r=0.9999),平均回收率为99.1%,RSD=1.5%(n=6)。结论所用方法操作简便,结果准确可靠。     

气相色谱法测定丁香油中丁香酚含量

目的建立气相色谱法测定丁香油中丁香酚含量的方法。方法以PEG-20M弹性石英毛细管柱（25m×0．20mm×0．33μm）为固定相,FID检测器,柱温175℃,载气为氮气,流速lml·rain～。结果丁香酚进样量在0．2054μg-2．054μg范围内,其峰面积对其进样量呈良好线性关系。Y=0．9107X-0．625·10-1,r=0．9998,加样回收率为99．62％,RSD为1．23％（n=9）。结论该方法灵敏、简便,结果准确可靠,可作为控制丁香油质量的方法。     

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.     

HPLC法测定麻仁丸中大黄素和大黄酚的含量

目的:建立麻仁丸中大黄素和大黄酚含量测定的方法。方法:色谱柱为Thermo ODS C18柱(250 mm×4．6 mm,5μm),流动相为甲醇-0．1％磷酸溶液(85:15),流速为1．0 ml·min-1,检测波长为254 nm。结果:大黄素在0．01-0．29μg(r =0.999 5);大黄酚在0．03-0．52μg(r=0．999 4)范围内线性关系良好。大黄素及大黄酚的平均回收率分别为100.4％(RSD =0．9,n=5),100．1％(RSD=0．3％,n=5)。结论:方法准确可靠。     

气相色谱法测定细辛脑中的有机溶剂残留量

目的 建立气相色谱法测定细辛脑中四氢呋喃、乙醇、甲苯的残留量。方法 采用SUPELCOWAX-10的毛细管石英色谱柱（30mm×0．53mm，1．0μm）；载气：氮气；以N，N-二甲基甲酰胺为溶剂；柱温：60℃，保持5min，以30℃·min^-1。升温至180℃，维持1min；进样口温度：250℃；检测器温度：250℃（FID）。结果 四氢呋喃在0．634～211．2μg·mL^-1内线性关系良好，r＝0．999 1 （n＝6），最低检测限为0．190μg·mL^-1，回收率为98．8％（RSD=4．3％）；乙醇在1．032～206．4μg·mL^-1内线性关系良好，r＝0．9992（n＝6），最低检测限为0．310μg·mL^-1,回收率为97．7％（RSD=3．O％）；甲苯在0．604～36．24μg·mL^-1内线性关系良好，r＝0．9995（n＝6）），最低检测限为0．174μg·mL^-1，回收率为100．3％（RSD＝0．7％）：结论本方法可用于细辛脑中四氢呋喃、乙醇和甲苯的残留量测定。     

气相色谱法测定冠心膏中樟脑、冰片和薄荷脑含量

目的探讨冠心膏中樟脑、冰片和薄荷脑含量的测定方法。方法采用气相色谱（GC）法，色谱柱为PEG-20M弹性石英毛细管色谱柱（30m×0．53mm×1μm），检测器为FID检测器。结果樟脑的线性进样量范围为0．095～0．95μg（r=0．9997，n=5），平均回收率为99．5％，RSD为1.9％；薄荷脑的线性进样量范围为0．123～1．23μg（r=0．9996，n=5），平均回收率为98．6％，RSD为2、0％；冰片的线性进样量范围为0．202—2．02μg（r=0．9997，n=5），平均回收率为99、4％，RSD为4．4％。结论GC法简便、快速、准确、重现性好，可以用于冠心膏的质量控制。     

顶空气相色谱法测定乙基纤维素中有机溶剂残留量

目的 建立乙基纤维素中残留有机溶剂二氯甲烷的测定方法。方法采用顶空进样毛细管气相色谱法,FID检测器。色谱柱为DB-624石英毛细管柱（30m×0．3mm,1．8μm）,载气为氮气,柱温90℃。结果二氯甲烷可得到有效分离,在所考察的质量浓度范围内线性关系良好,r=0．9996（n=6）,平均回收率为98．99％,RSD=1．04％（n=9）。结论所用方法灵敏、准确、快速,可作为乙基纤维素中残留有机溶剂二氯甲烷的检测方法。     

气相色谱法测定仁丹中薄荷脑含量

目的建立仁丹中薄荷脑的含量测定方法。方法采用气相色谱法,色谱柱为DB-Waxetr弹性石英毛细管柱（30m×0．32mm,1．0μm）,载气为N2,流速为1．5mL／min,柱温为140℃。结果薄荷脑进样量在0．02164-1．0820μg范围内与峰面积线性关系良好（r=0．9994）,平均加样回收率为100．72％,RSD为1．95％（n=6）。结论所用方法灵敏、简便、准确、重现性好,适用于仁丹的质量控制。     

卡马西平中残留溶剂的研究

目的:用气相色谱的顶空进样法建立卡马西平中的残留溶剂氯苯、甲醇和乙醇的测定方法.方法:使用配置顶空进样器的气相色谱仪,采用HP-INNOWAX(交联聚乙二醇),30m×0.32mm×0.25μm色谱拄,以氮气为载气,FID检测器,顶空进样.通过外标法计算残留溶剂的含量.结果:卡马西平中有残留溶剂甲醇、乙醇检出.标准曲线的线性范围:氯苯为0.07～3.62μg·mL-1(r=0.9992),甲醇为0.60～30.1μg·mL-1(r=0.9978),乙醇为1.00～50.08μg·mL-1(r=0.9986),定量限氯苯为0.1μg·mL-1,甲醇为0.7μg·mL-1,乙醇为0.4μg·mL-1;平均回收率氯苯为99.12%(RSD=2.52%,n=6),甲醇为97.51%(RSD=4.31%,n=6),乙醇为98.52%(RSD=3.12%,n=6).结论:本方法简便,灵敏度高,重复性好,结果准确.     

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.