高效液相色谱法测定逍遥丸中芍药苷的含量

目的　建立逍遥丸 (浓缩丸 )中芍药苷的含量测定方法。 方法 　高效液相色谱法 Kromasil KR10 0 5 C1 8色谱柱 ( 2 5 0× 4.6mm)流动相 :乙腈 -水 ( 2 0∶ 80 ) :流速 :1.0 m L· min- 1 ;检测波长 :2 3 0 nm。结果 　芍药苷进样量在 0 .2 2 2～ 1.77μg范围内呈良好的线性关系。 ( r=0 .99997,n=6) ,重复性良好 ,RSD=1.3 %( n=6) ,平均回收率 97.9%,RSD=0 .8%( n=6)。 结论　本法快速、简便、准确、重复性好。     

RP-HPLC测定异烟肼片的含量

目的　建立了反相RP -HPLC测定异烟肼片含量的方法。方法　选用C18色谱柱 (5 μm ,2 5 0mm× 4 6mm) ,以甲醇 -水 -冰醋酸 (4 4∶5 5∶1)为流动相 ,流速 0 9ml·min-1,紫外检测波长为 2 6 3nm ,尼可刹米为内标。结果异烟肼在 10～ 12 0 μg·ml-1,面积比与其浓度线性关系良好 (r=0 9999) ;样品平均回收率为 99 8% ,RSD =0 6 7% (n =5 )。结论　方法准确、快速、简便 ,且不受辅料干扰     

高效液相色谱法测定齐多夫定胶囊中AZT的含量

目的 　建立齐多夫定胶囊中 AZT的含量测定方法。方法 　高效液相色谱法 ,Nova-Pak○RC1 8色谱柱 ( 60 A0 4μm,3 .9× 15 0 mm) ;流动相 :甲醇 -水 ( 2 0∶ 80 ) ;流速 :1.0 m L· min- 1 ;检测波长 :2 65 nm。 结果　齐多夫定进样量在 0 .2～ 2 .0 μg范围内呈良好的线性关系 ( r=1.0 0 0 0 ,n=5 ) ,重复性良好 ,RSD=0 .96% ( n=6) ,平均回收率 10 0 .1% ,RSD=1.49% ( n=9)。 结论　本法快速、简便、准确、重复性好     

HPLC法同时测定尿多酸肽注射液中4-羟基苯乙酸及5-羟基吲哚乙酸的含量

目的　以HPLC法同时测定尿多酸肽注射液中4 - 羟基苯乙酸及5 - 羟基吲哚乙酸的含量。方法　采用MightysilRP C1 8(2 5 0mm×4 . 6mm ,5 μm)色谱柱,以1 %的甲酸溶液为流动相A ,乙腈为流动相B ,梯度洗脱,柱温30℃,流量1ml·min-1 ,检测波长2 82nm。结果　4 羟基苯乙酸在1 .0～1 4 0 . 0 μg·ml-1 范围内,色谱峰面积与对照品浓度呈现良好的线性关系,r=1 . 0 0 0 ;平均回收率为1 0 0 . 7%(RSD为0 . 6 %,n =9)。5 羟基吲哚乙酸在0 .1～2 0 . 0 μg·ml-1 范围内,色谱峰面积与对照品浓度呈现良好的线性关系,r=1 . 0 0 0 ;平均回收率为99 .7%(RSD为0 .6 %,n =9)。结论　该方法灵敏度高,准确,选择性、重复性好。     

高效液相色谱法测定消银霜中丙酸氯倍他索的含量

目的 :建立消银霜中丙酸氯倍他索含量测定的高效液相色谱法。方法 :色谱柱为LichrospherC18柱 (5 μm ,4 .6mm×2 5 0mm) ;流动相 :甲醇 水 (80∶2 0 ) ;流速 :1.0mL·min-1;检测波长 :2 39nm。结果 :丙酸氯倍他索浓度在 19.94～ 99.6 8mg·L-1范围内与色谱峰面积呈良好的线性关系 (r =0 .9998) ,平均回收率为 99.90 % ,日内和日间RSD分别为 0 .8% (n =6 )和1.9% (n =5 )。结论 :高效液相色谱法测定消银霜中丙酸氯倍他索的含量测定方法操作简单 ,结果准确 ,重复性好。     

RP-HPLC法测定葛根素氯化钠注射液中葛根素的含量

目的 :测定葛根素氯化钠注射液中葛根素的含量。方法 :采用 RP- HPL C法测定 ,色谱柱为 L una C1 8(15 0 mm× 4 .6 mm,5 μm) ,流动相为甲醇 -水 (2 8∶ 72 ) ,检测波长为 2 5 0 nm。结果 :葛根素对照品在 5～ 5 0 μg/ ml范围内线性关系良好 ,r =0 .9999(n =6 ) ,平均回收率为 99.82 % ,RSD为 0 .6 2 % (n =15 )。结论 :本方法操作简便、准确、重复性好 ,可作为该制剂的定量分析方法。     

氧氟沙星胶囊含量测定HPLC法的改进

目的　采用HPLC法改进的流动相系统测定氧氟沙星胶囊中氧氟沙星的含量。方法　色谱柱 :TechsphereC1 8ODS柱(1 5 0mm× 4 6mm ,5 μm) ,流动相 :0 0 5mol·L-1 枸橼酸 -乙腈 -四乙胺 (70∶2 8∶2 ) ,流速 :0 8ml·min-1 ,UV检测波长 :2 93nm。结果　氧氟沙星在 2 0 4～ 1 0 2 0mg·L-1 范围内 ,浓度与峰面积线性关系良好 (r =0 9999) ,日内RSD =1 0 7% (n =5 ) ,日间RSD =1 2 3% (n =3)。平均回收率为 99 98% (n =5 )。结论　改进后方法简便、快速、结果准确 ,可用于氧氟沙星胶囊的质量控制     

RP-HPLC测定替拉扎明及其有关物质

目的　建立测定替拉扎明含量及其有关物质检查的高效液相色谱法。方法　采用HypersilC18色谱柱(2 5 0mm× 4.6mm ,id 10 μm) ,甲醇 - 5 0mmol·L-1磷酸盐缓冲液 (10∶90 ,氢氧化钠调pH =6 .5± 0 .1)为流动相 ,在检测波长 2 6 6nm处进行含量测定 ;在相同条件下 ,以甲醇 - 5 0mmol·L-1磷酸盐缓冲液 (2 5∶75 ,氢氧化钠调pH =6 .5±0 .1)为流动相 ,对有关物质进行检查。结果　替拉扎明在 1.2 7～ 5 0 .8μg·ml-1范围内 ,峰面积与其浓度线性关系良好 (r =0 .9999) ,最低检测限为 2 .5× 10 -2 ng (S/N =3) ,重复进样RSD =0 .6 9% (n =5 ) ,日内RSD =0 .83%(n =5 ) ,日间RSD =0 .39% (n =5 ) ,重复性试验RSD =0 .2 1% (n =6 ) ,加样回收率为 99.6 2 %。结论　本法准确、简便、快速 ,可用于替拉扎明原料药及其制剂的质量控制     

HPLC测定磷酸咯萘啶片中主药的含量

目的　建立测定磷酸咯萘啶含量的HPLC方法。方法　选用DiamonsilC1 8(2 50mm× 4 .6mm ,5μm)色谱柱 ,0 .0 8mol·L- 1 磷酸二氢钾 -乙腈 (85∶1 5)为流动相 (含 0 .1 %三乙胺 ,pH3 .0 ) ;检测波长 2 78nm ;流速为 1 .0ml·ml- 1 ;进样量 2 0 μl。 结果　磷酸咯萘啶在浓度 5 .0 8～ 40 6 .4μg·ml- 1 范围内线性关系良好 ;回归方程为A =- 1 2 91 8+1 8657C ,r =0 .9999;平均回收率为 99.8% ,RSD =0 .8% (n =5)。结论　本法简便、灵敏、准确     

高效液相色谱法测定口炎Ⅱ号冲剂中栀子苷的含量

目的　测定口炎 号冲剂中栀子苷的含量。 方法 　高效液相色谱法 ,ODS柱 (4 .0× 2 5 0 mm,5μm) ;流动相 :CH3CN-H2 O(13∶ 87) ;流速1.0 ml· min- 1 ;检测波长 :2 80 nm ,柱温 :3 0℃。结果 　栀子苷进样量在 0 .5～ 2 .5μg范围内呈良好线性关系 (r=0 .9989,n=5 ) ,重复性良好 ,RSD= 0 .8% (n=6) ,平均回收率 97.0 % ,RSD=0 .3 % (n=6)。 结论 　本法快速、简便、准确 ,重现性好。     

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.     

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.     

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.