HPLC法测定复方虎杖颗粒中盐酸小檗碱含量

目的 建立复方虎杖颗粒中盐酸小檗碱的含量测定方法。方法 采用反相高效液相色谱法,Alltima C₁₈(4.6 mm×250 mm,5 μm),流动相为乙腈-0.1%磷酸水溶液(50:50)(每100 mL加十二烷基磺酸钠0.1g),流速为1 mL.min_-1;检测波长为265 nm。结果 盐酸小檗碱在0.046～0.460 μg范围内与峰面积线性关系良好(r=0.999 9),平均回收率为100.79%,RSD为2.6%(n=6)。结论 该方法快速、准确、重现性好,可用于复方虎杖颗粒中盐酸小檗碱的含量测定。     

反相高效液相色谱法测定复方黄柏酊中小檗碱含量

目的建立复方黄柏酊中小檗碱的含量测定方法。方法用中性氧化铝吸附法制备样品,采用反相高效液相色谱法测定含量,色谱柱为C18柱(200mm×4.6mm,5μm),柱温为25℃,流动相为水-乙腈-磷酸二氢钾-十二烷基硫酸钠(50∶50∶0.3∶0.2),流速为1.0mL/min,检测波长为345nm。结果盐酸小檗碱浓度在50～250μg/mL范围内与峰面积线性关系良好,回归方程为A=46680.1C-154.0,r=0.9998(n=5),平均回收率为99.06%,RSD=0.19%。结论该方法灵敏、准确,重现性好,可作为复方黄柏酊中小檗碱的质量控制标准。     

HPLC测定脂溶性前列安栓中盐酸小檗碱的含量

目的 建立一种简便的测定脂溶性前列安栓中盐酸小檗碱含量的方法.方法 采用高效液相色谱法(HPLC)测定盐酸小檗碱的含量.色谱条件为Kromasil C18 柱( 4.6 mm × 200 mm,5 μm), 流动相为乙腈-0.1%磷酸溶液(50:50)(每100 ml中加入十二烷基硫酸钠0.1 g ),检测波长350 nm.供试品预处理采用超声溶解法.结果 盐酸小檗碱在20～200 μg·ml-1范围内有良好的线性关系(r=0.9999),平均回收率为98.9%,RSD为0.5%.结论 本方法可用于脂溶性前列安栓中盐酸小檗碱的含量测定,方法简便、快速、灵敏.     

TLCS法测定复方黄连颗粒中盐酸小檗碱的含量

目的建立复方黄连颗粒中盐酸小檗碱含量TLCS测定方法。方法采用TLCS法,展开剂为正丁醇-冰乙酸-水(5∶1∶1),检测波长为345 nm。结果盐酸小檗碱在0.0912~0.2736μg性线范围内线性关系良好,相关系数r=0.998 6,平均回收率为100.80%,RSD=3.53%(n=5),制剂中盐酸小檗碱含量应不低于15.0%。结论该方法简单、结果准确、可作为该制剂的质量控制方法。     

HPLC法同时测定烫伤合剂中绿原酸、虎杖苷和盐酸小檗碱的含量

目的:建立烫伤合剂中绿原酸、虎杖苷和盐酸小檗碱含量的测定方法.方法:采用HPLC法,用色谱柱为Inertsil C8-3(250 mm×4.6 mm,5 μm)柱,乙腈-0.1%磷酸-四氢呋喃(19:80:1)为流动相,流速为1.0 ml·min-1,检测波长为290 nm.结果:绿原酸、虎杖苷和盐酸小檗碱的线性范围分别为25.45～254.5(r=0.999 4),3.07～30.75(r=0.999 6)和6.62～66.25 μg·ml-1(r=0.999 7);平均加样回收率分别为99.99%,97.40%和98.81%(n=6).结论:此法简便、准确,具有良好的重复性好,适用于烫伤合剂中3种组分的同时测定.     

复方芒果苷滴眼液中芒果苷和盐酸小檗碱的鉴别及含量测定

目的 采用TLC定性鉴别复方芒果苷滴眼液中的芒果苷和盐酸小檗碱并用HPLC测定其含量.方法 用C_(18)柱,流动相为乙腈-0.05 mol·L~(-1)磷酸二氢钾缓冲液(28:72),流速1.0 mL·min~(-1),检测波长265 nm,外标法定量.结果 芒果苷和盐酸小檗碱的线性范围均为0.1～1.0 μg,平均回收率分别为101.0%(RSD=2.09%,n=9)、100.6%(RSD=1.87%,n=9).结论 所建方法简便、准确,可用于复方芒果苷滴眼液的质量控制.     

HPLC 测定黄连上清丸中盐酸小檗碱的含量

目的采用HPLC测定黄连上清丸中盐酸小檗碱的含量.方法以YWG-C18为固定相,乙腈-0.1 mol*L-1磷酸二氢钾溶液-0.025 mol*L-1十二烷基硫酸钠溶液(50∶25∶25)为流动相,检测波长265 nm.结果盐酸小檗碱线性范围为0.04344～1.086 μg,r=0.9999,平均回收率为98.6%(RSD=1.2%,n=6),方法精密度RSD＝1.5%(n=5).结论所用方法简便快速,结果准确.     

反相高效液相色谱法测定兔血浆中盐酸小檗碱的浓度

目的:建立血浆中盐酸小檗碱浓度的测定方法。方法:采用反相高效液相色谱内标法,色谱柱为DikmadiamonsilTMC18,流动相为乙腈-0.1mol/L磷酸二氢钾溶液-十二烷基硫酸钠(50∶50∶0.06),流速为1ml/min,检测波长为345nm,柱温为40℃,内标物为对二甲氨基苯甲醛。结果:盐酸小檗碱检测浓度在20.5～656ng/ml范围内线性关系良好(r=0.9999),平均回收率为99.14%,平均RSD为3.78%。结论:该方法灵敏度高、专属性强,可用于盐酸小檗碱的药动学研究。     

健脾止泻宁颗粒的质量标准提高研究

目的:提高健脾止泻宁颗粒的质量标准。方法:采用薄层色谱法(TLC)对制剂中黄芩、山楂、金银花、党参、莲子、黄连进行定性鉴别;采用高效液相色谱法测定制剂中盐酸小檗碱、黄芩苷的含量:色谱柱为Shimadzu VP-ODS,流动相为甲醇-乙腈-水(46∶30∶42,V/V/V,盐酸小檗碱)(含0.1%十二烷基磺酸钠和0.1%磷酸)、甲醇-0.4%磷酸溶液(50∶50,V/V,黄芩苷),流速为1.0m L/min,检测波长为265 nm(盐酸小檗碱)、280 nm(黄芩苷),柱温为30℃,进样量为10μL。结果:黄芩、山楂、金银花、党参、莲子、黄连的TLC图斑点清晰,分离度好,阴性对照无干扰。盐酸小檗碱、黄芩苷检测质量浓度线性范围分别为6.67~33.34μg/m L(r=0.999 8)、7.7~38.7μg/m L(r=0.999 9);精密度、稳定性、重复性试验的RSD<1.0%;加样回收率分别为96.5%~99.9%(RSD=1.2%,n=6)、101.1%~102.9%(RSD=0.6%,n=6)。结论:提高的标准可用于健脾止泻宁颗粒的质量控制。     

HPLC法测定复方小檗碱鞣酸蛋白胶囊中盐酸小檗碱的含量

目的:建立高效液相色谱法测定复方小檗碱鞣酸蛋白胶囊中盐酸小檗碱含量的方法。方法:采用CAPCELL PAK C18柱(250mm×4.6mm,5μm),以磷酸盐缓冲液[0.05mol/L磷酸二氢钾溶液-0.05mol/L庚烷磺酸钠溶液(1∶1),含0.2%三乙胺,并用磷酸调节pH值至3.0]-乙腈(60∶40)为流动相,流速1mL/min,检测波长263nm,柱温30℃。结果:盐酸小檗碱进样量在0.2016～2.4192μg范围内呈良好线性关系(r=0.9998),平均回收率100.6%,RSD=1.3%(n=9)。结论:本方法结果准确,专属性强,重现性好,可作为复方小檗碱鞣酸蛋白胶囊中盐酸小檗碱含量测定的方法。     

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.

---

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.