固相萃取-多波长超高效液相色谱法同时测定咳喘宁中5种生物碱类成分的含量

建立咳喘宁中罂粟壳和麻黄所含5种主要生物碱类成分的含量测定方法。样品经固相萃取后用超高效液相色谱法测定,色谱柱为Acquity UPLC BEH C18(100 mm×2.1 mm ID,1.7μm),流动相为乙腈与0.1%磷酸溶液梯度洗脱,检测波长为210 nm(吗啡、磷酸可待因、盐酸麻黄碱和盐酸伪麻黄碱)与251 nm(盐酸罂粟碱),流速0.4 mL·min-1,柱温30℃。结果显示,吗啡、磷酸可待因、盐酸罂粟碱、盐酸麻黄碱和盐酸伪麻黄碱分别在0.375 0～12.50、0.064 32～2.144、0.030 06～1.002、1.126～37.52、0.287 8～9.592μg·mL-1内具有良好的线性关系(r=0.999 7),平均回收率分别为(n=9)99.26%、100.6%、95.29%、100.1%和97.48%。该方法快速、准确、重复性好,可为咳喘宁的质量控制提供快速准确的检测。     

HPLC法同时测定桂灵片中6种生物碱的含量

目的：建立HPLC法同时测定桂灵片中6种生物碱的含量。方法：采用Agilent Eclipse Plus-C18色谱柱（4.6 mm×250 mm,4.6 μm）,以乙腈（A）-0.1%磷酸（B）为流动相,梯度洗脱,流速1.0 mL·min-1,测定波长：吗啡、盐酸麻黄碱、盐酸伪麻黄碱、盐酸甲基麻黄碱、磷酸可待因210 nm;盐酸罂粟碱251 nm。结果：吗啡、盐酸麻黄碱、盐酸伪麻黄碱、盐酸甲基麻黄碱、磷酸可待因和盐酸罂粟碱进样量分别在0.001 3～0.13 μg（r=0.999 9）,0.002 5～0.25 μg（r=0.999 9）,0.002 5～0.25 μg（r=0.999 9）,0.005 4～0.27 μg（r=0.999 9）,0.002 6～0.26 μg（r=0.999 9）,0.000 5～0.11 μg（r=0.999 9）范围内呈良好线性关系,平均回收率（n=6）分别为101.6%、100.2%、95.3%、99.2%、103.5%、100.2%。结论：该方法可以用于桂灵片的质量控制。     

HPLC法同时测定强力枇杷露中吗啡与可待因含量

目的 提高强力枇杷露的质量标准.采用高效液相色谱法对强力枇杷露中的吗啡与可待因进行含量的同时测定.方法 色谱柱为Agilent Eclipse C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.01 mol·L-1磷酸二氢钾-磷酸-三乙胺溶液(5∶95∶0.2∶0.4)为流动相,流速1.0 mL·min-1,检测波长220 nm.结果 吗啡的进样量在0.229 3～4.586 μg范围内呈良好的线性关系(r=0.999 2),平均加样回收率为100.35％,RSD为2.87％(n=6);可待因的进样量在0.037 11～0.741 1μg范围内呈良好的线性关系(r=0.999 9),平均加样回收率为106.78％,RSD为2.09％(n=6).结论 方法经济合理、简便准确,可用于强力枇杷露中吗啡和可待因的含量测定.     

HPLC法同时测定复方可待因口服溶液中磷酸可待因、盐酸麻黄碱、盐酸曲普利啶的含量

目的 建立同时测定复方可待因口服溶液中磷酸可待因、盐酸麻黄碱、盐酸曲普利啶3组分含量的高效液相色谱法。方法 采用Hypersil-BDS CN柱,流动相为乙腈-0.4％乙酸铵溶液-三乙胺(30:70:0.2),流速为1.0 ml/min,检测波长257nm,外标法计算。结果 线性范围分别是磷酸可待因125-1 000 μg/ml,r=0.9999,盐酸麻黄碱75-600μg/ml,r=0.9996;盐酸曲普利啶18-140 μg/ml,r=0.9997。回收率分别为磷酸可待因99.9％、盐酸麻黄碱99.7％、盐酸曲普利啶100.3％。结论 本方法分离效果好,辅料无干扰,快速,简便,适合于该制剂3组分的同时测定。     

HPLC法同时测定复方可待因口服溶液中磷酸可待因、盐酸麻黄碱、盐酸曲普利啶的含量

目的建立同时测定复方可待因口服溶液中磷酸可待因、盐酸麻黄碱、盐酸曲普利啶3组分含量的高效液相色谱法.方法采用Hypersil-BDS CN柱,流动相为乙腈-0.4%乙酸铵溶液-三乙胺(30:70:0.2),流速为1.0 ml/min,检测波长257nm,外标法计算.结果线性范围分别是磷酸可待因125～1 000μg/ml,r=0.9999,盐酸麻黄碱75～600μg/ml,r=0.9996;盐酸曲普利啶18～140 μg/ml,r=0.9997.回收率分别为磷酸可待因99.9%、盐酸麻黄碱99.7%、盐酸曲普利啶100.3%.结论本方法分离效果好,辅料无干扰,快速,简便,适合于该制剂3组分的同时测定.     

HPLC测定利咳定糖浆中磷酸可待因的含量

目的为了控制利咳定糖浆的质量,建立磷酸可待因的含量测定方法.方法采用HPLC测定利咳定糖浆中磷酸可待因的含量,流动相为甲醇:0.68%的磷酸二氢钾溶液(18∶82),用10%的磷酸调节pH=3.5,固定相为hypersil BDS C18(4.6 mm×250 mm,5 μm),流速1.0 ml/min,检测波长为224 nm.结果磷酸可待因在0.8864～7.0912 μg间有良好的线性关系,回收率为99.71%,RSD小于1.2%.结论方法简单,灵敏度高,可用于利咳定糖浆中磷酸可待因的含量测定.     

HPLC测定盐酸阿扑吗啡舌下片的有关物质

目的 采用HPLC测定盐酸阿扑吗啡舌下片的有关物质.方法 采用Dimasil C18柱(250 mm×4.6 mm,5 μm);乙腈-0.04 mol·L-1磷酸二氢钾溶液(磷酸调pH3)(2:8)为流动相;检测波长272 nm.结果 盐酸阿扑吗啡进样量0.8～12.4μg与峰面积的线性关系良好(r=0.9999);最低检测限为0.8 ng.结论 所建方法准确、简便、快速,适用于盐酸阿扑吗啡舌下片的质量控制.     

RP-HPLC同时测定复方甘草片中4个成分的含量

目的:采用高效液相色谱法同时测定复方甘草片中吗啡、磷酸可待因、甘草苷和甘草酸的含量。方法:采用PhenomenexLuna-C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.02 mol·L-1磷酸二氢钾溶液(磷酸调pH至4.0)为流动相,梯度洗脱,流速1.0 mL·min-1,检测波长为220 nm(0～23 min,检测吗啡和可待因)、254 nm(23～50 min,检测甘草苷和甘草酸),柱温为35℃。结果:4个成分的峰面积与浓度的线性关系良好(r>0.9999);加样回收率为98.0%～100.8%。结论:该方法可用于复方甘草片中吗啡、磷酸可待因、甘草苷和甘草酸4个成分的含量测定。     

高效液相色谱法测定复方磷酸可待因口服液中3种有效成分的含量

目的 建立高效液相色谱法测定复方磷酸可待因口服液盐酸麻黄碱、磷酸可待因、马来酸氯苯那敏的含量. 方法 采用高效液相色谱法,色谱柱:C18(250 mm×4.6 mm,5 μm);流动相:甲醇-水-三乙胺-高氯酸钠(650:350:2:2);检测波长:261 nm;流速:1.0 mL.min^-1;柱温:35 ℃;进样量:20 μL. 结果 盐酸麻黄碱在0.051～0.463 mg.mL^-1线性关系良好(r=0.999 9),平均回收率98.9%,RSD=0.63%;磷酸可待因在0.039～0.355 mg.mL^-1线性关系良好(r=1.000 0),平均回收率100.4%,RSD=0.95%;马来酸氯苯那敏在0.032～0.285 mg.mL^-1线性关系良好(r=0.999 9),平均回收率100.7%,RSD=0.93%. 结论 该方法 操作简单、准确,可同时测定复方磷酸可待因口服液盐酸麻黄碱、磷酸可待因、马来酸氯苯那敏的含量,有效控制处方质量.     

HPLC同时测定止嗽定喘丸中的盐酸麻黄碱及盐酸伪麻黄碱

目的 建立止嗽定喘丸中盐酸麻黄碱与盐酸伪麻黄碱的含量测定方法.方法 采用固相萃取技术处理样品,HPLC测定,色谱柱为Shim - pack VP - ODS C18(150mm×4.6mm,5μm),流动相为乙腈-0.1％磷酸溶液(5∶95),检测波长210 nm,流速1 mL· rain-l.结果 4.41～147.0 μg·mL-1盐酸麻黄碱、2.33 ～116.6 μg·mL-1盐酸伪麻黄碱与峰面积的线性关系良好(r=0.9999),回收率分别为100.02％、97.73％(n=9).结论　所用方法准确可靠、重复性好,可作为止嗽定喘丸的质量控制.     

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.     

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.