注射用头孢拉定聚合物测定方法的建立

目的：建立高效液相色谱法测定注射用头孢拉定聚合物的含量。方法：采用高效液相色谱法,色谱柱为TSK-GEL G2000SWXL凝胶色谱柱,流动相为pH 8.0的0.2 mol/L磷酸盐缓冲液即0.2 mol/L磷酸氢二钠溶液-0.2 mol/L磷酸二氢钠溶液（95∶5）,检测波长210 nm,柱温30℃,流速1 mL/min,进样量20μL。结果：头孢拉定对照品检测线性范围为5.21-208.57μg/mL（r=0.99997）,注射用头孢拉定聚合物检测线性范围为0.17-3.37 mg/mL（r=0.999）,聚合物定量限为0.14μg。结论：该方法测定注射用头孢拉定聚合物专属性好,快速,分离度好,可用于注射用头孢拉定聚合物的检测。     

HPLC法测定头孢克洛颗粒中头孢克洛及其异构体

目的 建立HPLC法测定头孢克洛颗粒中头孢克洛及其异构体。方法 采用P/NO．OOG-4435-EO Desc．Gemini 5μ C18 110A Size 250﹡4.60mm 5 micron S/NO．490274-28柱,柱温35℃;流动相A为0.78%磷酸二氢钠溶液,流动相B为0.78%磷酸二氢钠溶液(pH4.0)-乙腈(55：45);检测波长220nm;流速1.0mL.min-1;线性梯度洗脱。结果 最低检测限为1.02ng。结论 本方法灵敏、精密度高、专属性强,可用于头孢克洛颗粒中头孢克洛及其异构体。     

注射用头孢拉定有关物质Ⅱ考察方法研究

目的建立测定注射用头孢拉定中有关物质Ⅱ的高效液相凝胶色谱法。方法采用TSK G2000SWXL凝胶色谱柱(TOSOH,7.8mm×300mm),以磷酸盐缓冲液(p H7.0)[0.005mol/L磷酸氢二钠溶液–0.005mol/L磷酸二氢钠溶液(61:39)]-乙腈(95:5)为流动相,检测波长为254nm;流速为0.8m L/min。结果头孢拉定对照品溶液在0.4950~14.8450μg/m L范围内,溶液浓度和峰面积线性关系良好(r=1.0000)。重复性的RSD为2.8%(n=6)。结论本凝胶色谱方法操作简便,专属性强,结果可靠,可用于注射用头孢拉定中有关物质Ⅱ的测定。     

凝胶色谱法测定注射用头孢拉定的聚合物

目的:建立用Sephadex G-10凝胶色谱法分析注射用头孢拉定中高分子杂质(头孢拉定聚合物)的方法。方法:色谱柱:Sephadex G-10柱(300mm×15.0mm,40~120μm);流动相A:pH8.0的0.2mol·L-1磷酸盐缓冲液[0.2mol·L-1磷酸氢二钠溶液-0.2mol·L-1磷酸二氢钠溶液(95:5)];流动相B:超纯水;检测波长:254nm;进样量:100μL;流速:1.5ml·min-1。结果:头孢拉定聚合物在0.506~101.26μg·mL-1范围内线性关系良好(r=1.0)。结论:该方法能较好的分离头孢拉定与其聚合物,方法简便、灵敏、准确,满足质量控制的要求。     

普卢利沙星的HPLC测定

建立了HPLC法测定普卢利沙星的含量。采用Luna C8色谱柱，流动相为乙腈-0．02mol几磷酸二氢钠溶液(49：51)，检测波长275nm，平均回收率为99．6％，RSD为0．64％。     

HPLC测定黄连炉甘石洗剂中小檗碱的含量

采用反相高效液相色谱法测定黄连炉城石洗剂中小檗碱的含量，色谱条件是十八烷基硅烷键合硅胶为填料的色谱柱，检测波长为２７７ｎｍ，流动相为乙腈－０．０５ｍｏｌ／Ｌ磷酸二氢钠；方法回收率１００．８％，小檗碱在０．０３－０．１６μｇ范围内呈良好线性关系。方法准确、可用于该制剂的质量控制。     

HPLC法结合LC-MS法测定硫酸鱼精蛋白含量及肽段鉴定

目的:建立了一种同时测定硫酸鱼精蛋白中主成分纯度和含量的HPLC方法，并采用LC-MS法对肽段氨基酸序列进行鉴定。方法:HPLC方法采用的色谱柱为ThermoHypersil GOLD色谱柱(250 mm×4.6 mm, 5μm),流动相A为0.1 mol·L^-1磷酸二氢钠溶液(用磷酸调节pH至1.8),流动相B为乙腈-0.1 mol·L^-1磷酸二氢钠溶液(用磷酸调节pH至1.8)(6.5∶93.5),梯度洗脱，流速1.0 mL·min^-1,柱温55℃,紫外检测波长为214 nm,进样量100μL。LC-MS法先采用馏分收集方式对各肽段进行提取富集，然后液质联用采用Waters ACQUITY UPLC Peptide BEH C₁₈色谱柱(15 cm×0.21 cm, 1.7μm),流速为0.2 mL·min^-1,流动相A为0.1%甲酸溶液，流动相B为5%乙腈-0.1%甲酸溶液，梯度洗脱；Thermo Q-Exactive Plus, ESI离子源，阳离子检测模式，雾化电压为...     

高效液相色谱法检测止咳平喘中药制剂中违法添加的茶碱

目的 建立止咳平喘中药制剂中违法添加的茶碱的检测方法。方法 采用高效液相色谱法并结合二极管阵列紫外光谱检测，色谱柱为Agilent TC C18柱，流动相为甲醇-0．06mol／L磷酸二氢钠溶液（25：75），流速为1．0mL／min，检测波长为270nm。结果 茶碱进样量在0．11-4．28μg范围内与峰面积线性关系良好，r=0．9999，平均回收率为98．8％（n=6），RSD=1．4％，最低检测限为2．39ng。结论 HPLC法具良好的灵敏度和专属性，能对止咳平喘中药制剂中违法添加的茶碱进行准确的定性和定量检测。     

聚乙二醇化天花粉蛋白注射液中天花粉蛋白的HPLC测定

建立了HPLC法检测聚乙二醇化天花粉蛋白注射液中天花粉蛋白的含量。采用硅胶基TSK-G3000SW凝胶柱，0．02mol／L磷酸二氢钠溶液-0．15mol／L氯化钠溶液-95％乙醇（45：45：10）为流动相，检测波长222nm。天花粉蛋白在5～50μg／ml范围内线性关系良好。平均回收率为100．0％，RSD为1．8％。     

RP-HPLC同时测定复方地塞米松乳膏中地塞米松和氯霉素含量

目的：应用RP-HPLC法测定复方地塞米松孔膏中地塞米松和氯霉素含量。方法：采用RP-HPLC法,流动相为甲醇-0．34％磷酸二氢钠溶液(45：55),检测波长240nm,流速1．0ml／min。结果：地塞米松和氯霉素两者线性关系良好,平均回收率分别为99．97％、99．87％,RSD分别为0．17％、0．17％。结论：方法快速,准确,可作为该制剂的质量控制方法。     

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.     

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.