HPLC测定胃蛋白酶合剂中的橙皮苷

目的 采用HPLC法测定胃蛋白酶合剂中的橙皮苷.方法 色谱柱为C18 (200 mm×4.6 mm,5 μm);流动相为乙腈-冰醋酸-水(9:1:40);流速1.0 ml · min-1;检测波长284 nm.结果 橙皮浓度2.5 ～40.0 μg · ml-1与峰面积有良好线性关系(r=0.9997);平均回收率为100.9%(RSD=1.6%).结论 所建方法操作简便,稳定可靠,可用于测定胃蛋白酶合剂中的橙皮苷.     

HPLC测定茄尼醇的含量

目的 采用RP-HPLC法测定茄尼醇粗品中的茄尼醇.方法 色谱柱为PRONTOSIL 120-5-C18-ace-APS(250 mm×4.6mm,5 μm);流动相为甲醇-乙醇(40:60);流速1.0 ml · min-1,检测波长210 nm. 结果茄尼醇的线性范围为3.24～51.84 μg · ml-1 (r=0.9998),最小检出限为0.52 ng.茄尼醇的平均回收率为109.1%,RSD=0.95%;结论所建方法简便、快速、准确,适用于茄尼醇的含量测定.     

HPLC法同时测定复方槐花口服液中柚皮苷和黄芩苷的含量

目的:建立HPLC法同时测定复方槐花口服液中柚皮苷、黄芩苷的含量.方法:色谱柱:Agilent ZORBAX SB- C18(250 mm×4.6 mm,5 μm);流动相:乙腈-0.1%磷酸溶液(23:77);检测波长:280 nm;流速:1.0 ml·min-1;柱温:30℃.结果:柚皮苷和黄芩苷分别在0.194～1.742 μg·ml-1(r=0.999 5,n=5)和0.419～3.773 μg·ml-1(r=0.999 8,n=5)范围内与峰面积呈良好线性关系,平均加样回收率为100.06%,RSD为1.10%(n=6)和99.27%,RSD为1.43%(n=6).结论:HPLC法操作简便,结果准确,可用于复方槐花口服液的质量控制.     

HPLC同时测定美敏伪麻溶液中盐酸伪麻黄碱、马来酸氯苯那敏及氢溴酸右美沙芬的含量

目的 建立用HPLC同时测定美敏伪麻溶液中盐酸伪麻黄碱、马来酸氯苯那敏及氢溴酸右美沙芬含量的方法.方法 采用色谱柱:HYPERSIL C18(4.6 mm×200 mm,0.5 μm),以十八烷基键合硅胶为填充剂.流动相:0.0025 mol·L-1己烷磺酸钠甲醇溶液-水(含1.5%三乙胺)(53∶47)用磷酸调至pH3.0.检测波长:205 nm;流速:1 ml·min-1.结果 线性范围分别是盐酸伪麻黄碱5.48～274 μg·ml-1(r=0.99997,n=5);马来酸氯苯那敏0.43～21.4 μg·ml-1(r=1.0000,n=5);氢溴酸右美沙芬1.94～96.8 μg·ml-1(r=0.99998,n=5).结论 本法简单、快速、精确、重复性高,可作为产品的质量控制方法.     

HPLC测定复方苦参凝胶剂中苦参碱与辣椒碱的含量

目的:应用高效液相色谱法测定复方苦参凝胶剂中辣椒碱与苦参碱的含量.方法:采用WatersμBONDAPAK C18柱(3.9 mm×300mm,5 μm),乙腈-0.05 mol·L-1磷酸二氢钠溶液-三乙胺(50:50:0.05);用磷酸调整pH值至2.2为流动相;检测波长为227 nm;流速:1.0 ml·min-.结果:辣椒碱线性范围为6.25～200μg·ml-1(r=0.999 9,n=5);苦参碱线性范围为80.0～800.0 μg·ml-1(r=0.999 7,n=5).辣椒碱平均回收率为101.8%(n=9),RSD=1.8%;苦参碱平均回收率为100.7%(n=9),RSD=0.9%.结论:本方法用于凝胶剂中辣椒碱与苦参碱含量的测定简便、快速、灵敏、结果准确.     

高效液相色谱法测定盐酸罂栗碱注射液的含量及有关物质

目的:采用高效液相色谱法测定盐酸罂粟碱注射液的含量及有关物质。方法:采用 C_(18)色谱柱(150 mm×4.6 mm,5 μm);流动相为0.5%醋酸铵-1%三乙胺-甲醇(39:1:60);流速1 mL·min~(-1);检测波长238 nm;柱温40℃。结果:盐酸罂粟碱的线性范围为10～160 μg·mL~(-1)(r=0.9999),平均回收率为99.86%(n=9);各杂质峰与主峰达到基线分离。结论:本方法简便、快速,结果准确,重复性好。     

HPLC法测定呋柳散中苯甲酸及水杨酸的含量

目的:建立HPLC法测定呋柳散中苯甲酸及水杨酸的含量.方法:色谱柱:依利特Hypersil C18(200 mm×4.6 mm,5 μm);流动相:甲醇-0.1mol·L-1磷酸二氢钠溶液(52:48);检测波长240 nm;流速为1.0 ml·min-1;柱温:室温.结果:水杨酸、苯甲酸在5.0～25.0 μg范围内线性关系良好(r=0.999 9),水杨酸平均回收率为99.32%(RSD=0.3%,n=9),苯甲酸平均回收率为99.48%(RSD=0.2%,n=9).结论:该方法专属性好,准确度高,重复性好.     

双波长HPLC法同时测定止痢宁片中穿心莲内酯和脱水穿心莲内酯的含量

目的:建立高效液相色谱法同时测定止痢宁片中穿心莲内酯和脱水穿心莲内酯含量的方法.方法:色谱柱:CAPCELL PAK-C18柱(150 mm×4.6 mm,5 μm);流动相:甲醇-水(48:52);流速为1.0 ml·min-1;柱温:30℃;检测波长:225 nm(穿心莲内酯)、250 nm(脱水穿心莲内酯);进样量:5 μl.结果:穿心莲内酯在4.17～41.68 μg·ml-1 (r=0.999 9)、脱水穿心莲内酯在4.04～40.40 μg·ml-1(r=0.999 9)浓度范围内线性关系良好;穿心莲内酯回收率为99.21%(RSD=1.3%,n=6),脱水穿心莲内酯回收率98.73%(RSD=1.1%,n=6).结论:该方法简单、准确,可作为止痢宁片的质量控制.     

餐时血糖调节剂米格列奈钙的RP-HPLC法人肝微粒体药物浓度测定

目的:建立人肝微粒体中米格列奈的高效液相色谱测定法.方法:采用Diamonsil-C18色谱柱(200 mm×4.6 mm,5μm);流动相为乙腈-0.02 mol·L-1KH2PO4缓冲液(pH 4.0)(43:57);流速为1.0 mL·min-1;紫外检测波长为210 nm;进样量为20 mL.结果:米格列奈最低检测限为2 μmol·L-1;线性范围为5～1 000 μmol·L-1(r=0.999 9);最低定量浓度为5μmol·L-1(RSD<5%,n=5);低、中、高3种浓度日内、日间RSD(n=5)分别为1.9%,1.6%,1.4%和3.8%,4.0%,3.8%;绝对回收率平均为94.4%,相对回收率平均为101.2%.结论:本实验建立的人肝微粒体中米格列奈的高效液相测定方法操作简便、结果准确.     

高效液相色谱法测定复方甲硝唑乳膏中甲硝唑和乳酸环丙沙星的含量

目的:建立复方甲硝唑乳膏中甲硝唑和乳酸环丙沙星含量测定的HPLC法.方法:采用Waters Symmetry C18色谱柱(250 mm×4.6 mm,5 μm),流动相为0.05 mol·L-1枸橼酸(三乙醇胺调pH至3.5)-乙腈(82:18),检测波长为287 nm,流速为1.0 ml·min-1.结果:甲硝唑浓度在20.0～100.0 μg·ml-1范围内与峰面积呈良好的线性关系(r=0.999 9),平均回收率为98.3%RSD为0.7%(n=5);乳酸环丙沙星浓度在16.0～80.0 μg·ml-1范围内与峰面积呈良好的线性关系(r=0.999 9),平均回收率为98.6%,脚%为0.9%(n=5).结论:方法简便、快捷,结果准确,适用于该制剂的质量控制.     

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.     

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.