高效液相色谱法测定中药升麻中阿魏酸和异阿魏酸的含量

目的 :测定中药升麻中阿魏酸和异阿魏酸的含量。方法 :反相高效液相色谱法。HypersilODS分析柱(2 5 0mm× 4 6mm ,5 μm) ,流动相 :甲醇 -水 -磷酸 (5 0∶15 0∶0 1) ,紫外检测波长 :32 0nm ,灵敏度 :1 0AUFS ,柱温 :2 4℃ ,流速 :1mL·min-1。结果 :阿魏酸在 0 0 42～ 2 10 μg (r =0 9993) ,异阿魏酸在 0 0 43～ 2 14μg (r =0 9994)范围内呈线性 ,阿魏酸和异阿魏酸平均回收率 (n =5 )分别为 98 76 % (RSD =1 6 % )和 98 32 % (RSD =1 8% )。结论 :本方法简便、精确、可靠。     

RP-HPLC测定普藏红胶囊中阿魏酸的含量

目的 :建立普藏红胶囊中阿魏酸含量的RP HPLC测定法。方法 :胶囊内容物先用 2 %碳酸钠水溶液提取 ,乙醚脱脂 ,然后用盐酸调pH1,再用乙醚提取出阿魏酸。在 μBondapakODS柱上分析 ,流动相为甲醇 水 (2 0∶80 ,磷酸调pH3.0 ) ,波长 30 0nm处检测 .结果 :阿魏酸在 10～ 5 0 μg·ml-1范围内 ,峰面积与浓度成良好线性关系 (r =0 .9998) ,加样回收率为 99.6 9% ,重复进样RSD为 0 .87% (n =5 ) ,重复性试验RSD为 1.14% (n =6 )。结论 :该法简便 ,快速 ,准确 ,适合于当归药材及其制剂中阿魏酸的含量测定     

HPLC测定高原雪灵芝中阿魏酸的含量

目的 :建立测定高原雪灵芝中阿魏酸含量的高效液相色谱法。方法 :采用碱液浸取、加酸沉淀后再用乙醚提取雪灵芝中的阿魏酸 ;色谱柱为 μBondapakODS柱 ,流动相为甲醇 水 冰醋酸 ( 4 0∶60∶3 ) ,检测波长 3 0 5nm。 结果 :雪灵芝中的阿魏酸与样品中其它成分分离良好 ;阿魏酸在 90～ 80 0 μg·ml-1范围内 ,峰面积与浓度的线性关系良好 (r=0 9997) ;平均回收率为 99 5 9%;日内精密度RSD =0 79%(n =5 ) ,日间精密度RSD =0 86%(n =5 )。结论 :该法操作简便 ,结果准确 ,可供生药材质量控制     

三维HPLC法同步测定犬血浆中的葛根素及阿魏酸

以对 羟基苯甲酸为内标 ,甲醇 水 醋酸 (5 6 2 5mol/L ) (39∶5 8∶3 ,v/v)为流动相 ,InertsilODS 3色谱柱 (15 0mm× 4 6mm ,5 μm)为固定相 ,流速 0 9mL/min。以二极管阵列检测器同时获取 2 48nm和 32 1nm两个波长下的数据 ,并通过三维图观察其紫外吸收定性 ,以沸水浴法处理血浆样品。结果 :葛根素和内标及阿魏酸分离完全 ,葛根素在 0 2 35 4～ 1 883μmol/L范围内线性关系良好 (r =0 9943) ,变异系数 <10 % ,平均回收率为 10 1 0 2 % ,最低检测限为 0 33ng ,最低检测浓度为 0 0 396 μmol/L;阿魏酸则在 1 0 341～ 5 35 6 μmol/L范围内线性关系良好 (r =0 9942 ) ,变异系数 <10 % ,平均回收率为 10 0 88% ,最低检测限为 0 45ng ,最低检测浓度为1 115 9μmol/L。此法可用于不同波长下同步以内标法测定血浆中两种或多种成分     

RP-HPLC法测定当归四逆颗粒中阿魏酸的含量

目的　建立RP HPLC测定当归四逆颗粒中阿魏酸的定量方法。方法　以反相高效液相法测定阿魏酸的含量。固定相 :ShimpackCLC_ODS(150mm× 6mm) ;流动相 :含 0 2 %甲醇的乙腈 含 0 1%磷酸和 0 1%三乙胺水溶液 (2 0∶80 ) ;检测波长 3 2 4nm。结果　阿魏酸在 1 2 4～ 2 4 80 μg/ml范围内线性良好 (r =0 9998) ,平均加样回收率为 98 7% ,RSD为 1 7%。 结论　定量方法简便 ,准确 ,能有效地控制当归四逆颗粒剂的质量     

高效液相色谱法测定阿魏酸血浆浓度

目的 建立测定血浆中阿魏酸浓度的高效液相色谱法。 方法 固定相为NucleosilC18柱 ,流动相为甲醇 -水 -冰乙酸 (35∶6 5∶0 1) ,流速 1 0ml·min-1,检测波长 32 0nm。以替硝唑为内标 ,血浆样品酸化后用乙酸乙酯提取。峰高比定量。 结果 标准曲线线性范围 0 5～ 16 0 μg·ml-1,γ =0 9995 ,阿魏酸平均回收率 96 9%～ 10 0 6 % ,最低检测浓度 0 2 μg·ml-1,日内RSD <3 0 % ,日间RSD <5 4%。 结论 本方法简便 ,快速 ,准确 ,重现性好 ,适用于阿魏酸血药浓度测定及药代动力学研究     

芪英愈疡颗粒中阿魏酸的HPLC测定

应用 HPL C法测定芪英愈疡颗粒中阿魏酸的含量。采用 YWG C1 8(2 5 0× 4.6 mm ,5μm)色谱柱 ,流动相 :甲醇 - 0 .0 6 6 mol/ L 磷酸氢二钠溶液 (以磷酸调 p H至 2 .5 ) (4 0∶ 6 0 ) ,流速 :1.0 ml/ min,检测波长 :32 0 nm,柱温 :室温。阿魏酸的线性范围为 0 .0 8～ 0 .32 μg,方法平均回收率为 98.9% ,RSD为 1.5 4%。     

RP-HPLC法测定复方甲硝唑片中甲硝唑和维生素B_6的含量

目的 :建立RP HPLC法测定复方甲硝唑片中甲硝唑和维生素B6的含量。方法 :采用Shim packCLC ODS柱 (4 .6mm× 2 0 0mm ,5 μm) ,甲醇 水 (30∶70 )为流动相 ,2 90nm为检测波长 ,外标法测定含量。 结果 :甲硝唑和维生素B6的线性范围分别为 5 0～ 5 0 0 μg·ml-1(r=0 .9996 ) ,5～ 5 0 μg·ml-1(r =0 .9998) ,平均回收率分别为 10 0 .2 % (RSD =0 .93% ) ,99.5 %(RSD =0 .4 2 % ) ,n =6。结论 :RP HPLC法测定复方甲硝唑片中甲硝唑和维生素B6的含量 ,方法准确 ,操作简便 ,结果可靠。     

咪唑斯汀缓释片稳定性分析法--HPLC法

目的 :建立咪唑斯汀缓释片的稳定性分析方法。方法 :采用高效液相色谱法。色谱柱为PhenomenexprodigyODS3 (2 5 0mm× 4 6mm ,5 μm) ;流动相 :甲醇 pH 4 0缓冲液 (7∶3) ;检测波长 2 80nm ;流速 1 0mL·min-1;外标法峰面积定量。结果 :咪唑斯汀保留时间约为 8 6min ,中间体、辅料、分解产物等对主药测定无干扰 ;咪唑斯汀浓度在 3～ 2 4 μg·mL-1范围内线性关系良好 ,回归方程为A =10 0 0 38 0 5C +6 5 5 6 ,r =0 99999;最低检出浓度为6 0ng·mL-1;日内、日间精密度 (RSD)分别为 0 39% (n =5 )和 0 5 6 % (n =5 ) ,重现性试验RSD =0 5 6 % (n =9) ;方法平均回收率为 99 4 7%～ 10 1 97% (n =5 ) ;模拟制剂平均回收率为 10 0 0 4 % (n =9)。结论 :该法灵敏、准确、专属性强 ,可用于咪唑斯汀片的稳定性研究。     

高效液相色谱法测定复方替硝唑搽剂中替硝唑和水杨酸的含量

目的 :建立测定复方替硝唑搽剂中替硝唑和水杨酸含量的高效液相色谱法。方法 :采用反相ODS色谱柱 ,甲醇 - 0 0 2mol·L-1KH2 PO4 溶液 (5 0∶5 0 )为流动相 ,检测波长为 315nm。结果 :替硝唑和水杨酸的线性范围分别在5 0～ 35 0 μg·mL-1(r=0 9997) ,40 0～ 16 0 0 μg·mL-1(r =0 9997) ;加样回收率分别为 10 0 6 % (RSD =0 6 9% )及 10 0 6 % (RSD =0 79% ) ;日内RSD为 0 16 %～ 1 2 %和 0 6 1%～ 1 2 % ,n =12 ,日间RSD为 0 2 4%～ 1 7%和0 2 %～ 1 1% ,n =4。结论 :HPLC法可用于复方替硝唑搽剂的含量测定 ,方法准确、灵敏 ,专属性强     

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.     

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.