HPLC测定毛兰素乳液型注射液中毛兰素及有关物质含量

目的 建立一种测定一类新药毛兰素乳液型注射液中毛兰素及有关物质鼓槌联苄含量的方法。方法 采用Agilent XDB C18柱(4.6 mm×250 mm,5 μm),流动相为甲醇-乙腈-水(30∶30∶40),检测波长：232 nm;流速：1.0 mL·min^-1。结果 毛兰素及有关物质鼓槌联苄达到完全分离;毛兰素在5.562 5~89.0 μg·mL-1内线性关系良好(Y=13 504X+2 146.6,r=0.999 9),平均回收率100.8%;有关物质鼓槌联苄在9.292~46.462 μg·mL^-1内亦有良好线性关系(Y=14.033 1X+2.388 6,r=0.999 9),平均回收率达99.8%。结论 本法灵敏,准确,专属性强,可用于测定注射液中毛兰素的含量和有关物质的检查。     

HPLC测定毛兰素乳液型注射液中毛兰素及有关物质含量

目的建立一种测定一类新药毛兰素乳液型注射液中毛兰素及有关物质鼓槌联苄含量的方法。方法采用AgilentXDBC18柱（4.6mm×250mm,5μm）,流动相为甲醇-乙腈-水（30∶30∶40）,检测波长：232nm;流速：1.0mL·min-1。结果毛兰素及有关物质鼓槌联苄达到完全分离;毛兰素在5.5625~89.0μg·mL-1内线性关系良好（Y=13504X＋2146.6,r=0.9999）,平均回收率100.8%;有关物质鼓槌联苄在9.292~46.462μg·mL-1内亦有良好线性关系（Y=14.0331X＋2.3886,r=0.9999）,平均回收率达99.8%。结论本法灵敏,准确,专属性强,可用于测定注射液中毛兰素的含量和有关物质的检查。     

叠鞘石斛与药典品种石斛酚含量对比研究

目的:建立叠鞘石斛与药典收载品种金钗石斛,鼓槌石斛中石斛酚的高效液相色谱含量测定方法。方法:DiamonsilCl8(150mm×4.6mm,5μm)色谱柱,乙腈-0.5%冰醋酸(35:65)为流动相,检测波长280nm,流速1mg.mL-1,柱温30℃。结果:石斛酚在0.01228~0.2456mg.mL-1(r=0.9999)范围内与峰面积线性关系良好,平均回收率为100.39%,RSD为2.17%。结论:本方法操作简单、快捷、重现性好、准确率高,可用于上述三种石斛中石斛酚的含量测定。     

铁皮石斛药材含量和检查项方法优化及不同产地品质的比较

目的 优化药典中甘露糖含量测定及甘露糖与葡萄糖面积比的色谱条件,同时比较浙江省不同产地铁皮石斛药材质量,为铁皮石斛适宜产地的选择提供依据。方法 以中国药典2010年版中铁皮石斛甘露糖含量测定方法为基础,对色谱条件进行优化,并用优化后的方法对不同产地铁皮石斛药材质量进行分析比较。结果 优化后的色谱条件：Diamonsil C₁₈(250 mm×4.6 mm,5 μm),以乙腈(A)-0.02 mol·L^-1的乙酸铵溶液(B)为流动相,梯度洗脱(0~60 min,14%A;60~61 min,14%→25%A;61~69 min,25%;69~70 min,25%→14%A;70→80 min,14%A),流速为1.0 mL·min^-1,检测波长为250?nm,柱温为30 ℃,进样量为10 μL。优化后的方法实现了PMP(1-苯基-3-甲基-5-吡唑啉酮)与甘露糖,PMP与样品杂质,盐酸氨基葡萄糖与样品杂质的基线分离。浙江省不同产地铁皮石斛药材在甘露糖含量及检查项比值上有一定的差异,其中富阳铁皮石斛的甘露糖含量最高,为40.8%,萧山铁皮石斛甘露糖与葡萄糖比值最高,为3.9。结论 该方法重复性好,结果准确可靠,可以用于铁皮石斛药材的质量控制。浙江省内不同产地的铁皮石斛质量存在一定的差异,其中建德最适宜人工栽培。     

HPLC法测定羟苯乙酯的含量

目的 用高效液相色谱(HPLC)法测定羟苯乙酯的含量.方法 色谱柱为C18柱(Agilent ZORBAX SB-C18,4.6 mm×150 mm,5 μm);流动相为甲醇-1%冰醋酸溶液(65∶35);流速为1.0 ml/min;柱温25℃;检测波长254 nm;进样量10 μl.结果 该方法羟苯乙酯的线性范围为0.050～0.250 mg/ml,r=0.999 95(n=5);回收率为99.9%;RSD=0.2%.结论 该法操作简便,快速、准确、灵敏度高,重复性好,可用于羟苯乙酯的含量测定.     

泽泻中泽泻烯醇的鉴定和含量测定

目的 采用TLC法鉴别泽泻中的泽泻烯醇,并采用HPLC法测定含量.方法 色谱柱为DiamonsilTM C18(150mm×4.6mm,5μm);流动相为乙腈-水(70:30);流速1 mL·min-1;柱温30℃.结果 10批泽泻药材中均能检出泽泻烯醇;泽泻烯醇4.958～19.832 μg与峰面积的线性关系良好(r=0.9995),平均回收率为99.66%,RSD =1.18%.结论 所建方法简便、准确、重复性好,可完善泽泻药材的质控方法.     

鼓槌石斛中一新的联苄类化合物——鼓槌石斛素

从兰科鼓槌石斛(Dendrobium chrysotoxum)中分得一新的联苄类化合物,经光谱分析(UV,IR,MS,¹HNMR,¹³CNMR和DIFNOE),其结构确定为4-羟基-3,5,3',4'-四甲氧基联苄,命名为鼓槌石斛素。关键词鼓槌石斛;鼓槌石斛素;联苄类化合物。     

RP-HPLC测定羌活中的总阿魏酸

目的 采用HPLC法测定羌活中总阿魏酸的含量.方法 色谱柱为Phenomenex Luna C_(18) (150 mm×4.6 mm,5 μm);流动相为乙腈-0.085%磷酸溶液(17:83);流速1.0 mL·min~(-1);柱温35 ℃;检测波长316 nm.结果 阿魏酸0.0059～0.1181 μg与峰面积线性关系良好(r=0.9999),平均回收率为99.08%(RSD=1.71%,n=6).结论 所建方法简便、快捷、重复性好,可作为羌活药材中总阿魏酸的含最测定方法.     

HPLC测定盐酸氨基葡萄糖分散片的含量

目的 建立盐酸氨基葡萄糖分散片的含量测定方法.方法 采用高效液相色谱法,C8色谱柱(200 mm × 4.6 mm,5 μm);流动相为0.05%磷酸溶液(KOH调pH 3.0)-乙腈(60∶40);流速0.6 mL/min;检测波长195 nm;柱温30℃.结果 在0.06 ~ 1.5 mg/mL的浓度范围内,盐酸氨基葡萄糖浓度与峰面积呈良好的线性关系(r = 0.999 7);平均回收率为100.7%(n = 9,RSD = 0.41%).结论 本方法简单、准确,适用于盐酸氨基葡萄糖分散片的含量测定.     

HPLC-ELSD法测定柴胡中柴胡皂苷a、d的含量

目的采用高效液相色谱法测定柴胡中柴胡皂苷a、d的含量.方法采用Alltech C18 (4.6 mm×250 mm,5 μm)色谱柱,甲醇-乙腈-水-冰醋酸(18∶40∶42∶0.2)为流动相,流速1.00 ml/min,Alltech ELSD-500检测器,外标法定量.结果柴胡皂苷a在5.025～15.075 μg 范围呈线性,回收率为96.2%,RSD为1.43%(n=9);柴胡皂苷d在5.670～17.010 μg范围呈线性,回收率为95.0%,RSD为1.76%(n=9).结论本法简便可行,重现性好,可作为柴胡药材质量检测的方法.     

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.

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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.     

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.     

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.     

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.