加校正因子的主成分自身对照法同时测定非那雄胺片中2个杂质

目的：建立加校正因子的主成分自身对照法测定非那雄胺片中有关物质的含量。方法：CAPCELL PAK C₁₈色谱柱(4.6′250 mm,5 mm),流动相乙腈-水(45∶55),流速1.0 mL.min_-1,检测波长210 nm,进样量20 mL,柱温30℃。测定非那雄胺与杂质Ⅰ、Ⅱ的标准曲线方程,以斜率计算杂质相对于非那雄胺的校正因子,用相对保留时间确定各杂质的位置。结果：非那雄胺杂质Ⅰ、Ⅱ的相对保留时间分别为0.85与1.30,相对校正因子分别为2.40与0.69。结论：本方法可用于非那雄胺片中有关物质的定性及定量分析,采用加校正因子的主成分自身对照法可以更准确的反映其有关物质的含量。     

女金丸GC指纹图谱研究

目的 建立女金丸GC指纹图谱,为其质量评价提供依据。方法 采用气相色谱法,FID检测器,HP-5毛细管柱（30 m×0.25 mm,0.25 mm）,升温程序为初始温度50℃,保持1 min,以20℃·min^-1的速率升温至130℃,保持10 min;再以2℃·min^-1的升温速率升至180℃,保持10 min;进样口温度230℃,检测器温度250℃;分流进样,分流比10：1。通过《中药色谱指纹图谱相似度评价软件》（2012年版）建立女金丸的GC指纹图谱,并进行相似度计算。结果 共确定女金丸GC指纹图谱30个共有峰,通过对照品对比及高分辨质谱谱库检索推测出全部色谱峰,各批样品相似度均>0.95。结论 所建立的指纹图谱可用于女金丸的整体质量控制和评价。     

毛细管气相色谱法测定替米沙坦有机溶剂残留量

目的建立气相色谱法分别测定替米沙坦中残留有机溶剂甲醇、乙醇、丙酮、二氯甲烷、氯仿、乙二醇和二甲基甲酰胺。方法以DB624弹性石英毛细管柱为色谱柱（30m×0．53mm）．载气为氮气,采用氢火焰离子化检测器,进样1：2温度为200℃,检测器温度为250℃。顶空进样法采用程序升温（50℃,保持15min。以30℃·min^-1升至160℃,保持5min）,进样量1．0mL。直接进样法柱温为100℃．进样量1．0μL。结果3批样品中7种有机溶剂残留量均符合规定。结论本方法可测定替米沙坦中的有机溶剂残留量,方法简单准确。     

顶空气相色谱法测定注射用胸腺法新中5种有机溶剂残留量

目的 建立同时测定注射用胸腺法新中乙腈、二氯甲烷、醋酸乙酯、苯和苯甲醚5种有机溶剂残留量的顶空气相色谱法。方法 采用Agilent DB-624（30 m×0.53 mm×3 μm）毛细管色谱柱;火焰离子化检测器;进样口温度200℃;检测器温度250℃;载气为氮气;载气体积流量为2.0 mL·min^-1;分流比为10：1;升温程序：起始温度40℃,保持6 min,以8℃·min^-1的速率升温至90℃,保持2 min,再以20℃·min^-1的速率升温至200℃,保持5 min;采用顶空进样方式,顶空加热箱温度80℃,样品瓶平衡时间30 min。进行系统适用性、检测限（LOD）与定量限（LOQ）、线性关系和范围、加样回收率、精密度、稳定性、耐用性考察。结果 注射用胸腺法新中5种残留溶剂在各自线性浓度范围内与峰面积线性关系良好;平均加样回收率在95.7%~106.3%;精密度、稳定性、耐用性均符合要求。5批胸腺法新中均未检出5种有机溶剂。结论 建立的顶空气相色谱法操作简单、灵敏度和准确度高、重现性和耐用性好,可用于注射用胸腺法新中5种有机溶剂残留量的测定。     

毛细管气相色谱直接进样检测34种残留溶剂

目的：建立一种常用的气相色谱法分离检测ICH中规定的34种残留溶剂。方法：以DB-624弹性石英毛细管柱为色谱柱（75m×0．53mm×3．0μm），载气为氮气，采用氢火焰离子化检测器（FID），进样口温度为220℃，检测器温度为300℃，柱温采用程序升温（35℃保持18min；以5℃·min^-1升至45℃，保持8min；以5℃·min^-1升至80℃，保持3min；以5℃·min^-1升至150℃，保持2min；再以30℃·min^-1升至250℃，并保持5min），流速3mL·min^-1。以N-甲基吡咯烷酮为溶剂，进样体积为1μL。结果：34种有机溶剂均能得到很好的分离，分离度绝大多数均大于1．5。峰面积与浓度呈良好的线性关系，精密度良好。结论：本文气相色谱条件可用于常用的34种溶剂的分离与测定，方法简单准确。     

气相色谱法测定氢溴酸替格列汀中溴乙烷残留量

目的 建立氢溴酸替格列汀中遗传毒性杂质溴乙烷残留量的气相色谱（GC）检测方法。方法 采用迪马DM-624色谱柱（30 m×0.53 mm×3.0 μm）;电子捕获检测器（ECD）;程序升温：初始柱温40 ℃,保持3 min,以20 ℃/min升温至200 ℃,保持5 min;进样口温度：210 ℃;检测器温度：210 ℃;载气：氮气;分流比：3：1;进样量1 μL。结果 溴乙烷在0.75～6.75 μg/mL与峰面积呈良好的线性关系（r=0.999 7）,最低检测限为0.26 μg/mL。平均回收率为99.4%,RSD值为0.3%（n=9）。3批氢溴酸替格列汀样品中均未检测出溴乙烷。结论 该方法简便、准确,重复性好,适用于氢溴酸替格列汀中溴乙烷残留量的控制。     

GC法测定高哌嗪中乙二胺和哌嗪的残留量

目的 建立气相色谱法（GC）测定高哌嗪中杂质残留乙二胺和哌嗪。方法 采用GC法,色谱柱为CP-sil8 CB（30 m× 0.25 mm×0.50 μm）;进样口温度240℃;升温程序：60℃保持1 min,以5℃/min的速率升温至110℃,再以40℃/min的速率升温至200℃,保持3 min;检测器为氢火焰离子化检测器（FID）,检测器温度为250℃;载气为氮气;分流比为2∶ 1;进样方式为直接进样,进样量1 μL;体积流量：1 mL/min。结果 高哌嗪中乙二胺杂质和哌嗪杂质与主成分间均能有效分离,线性范围分别为20.2～161.7 μg/mL（r=0.999 8）,20.4～163.6 μg/mL（r=0.999 9）。重复性和精密度的RSD值均在规定范围内。结论 该方法适用于高哌嗪中乙二胺和哌嗪杂质的准确测定和质量控制。     

气相色谱法测定达比加群酯中10种溶剂的残留

目的：建立气相色谱法检测达比加群酯中10种残留溶剂。方法：以Rtx-1（60 m×0.32 mm×1.0μm）极性毛细管柱程序升温,以氮气为载气,FID 为检测器,进样口温度为 200℃,检测器温度为 250℃,对达比加群酯中 10种残留溶剂（甲醇、乙醇、乙酸乙酯、丙酮、二氯甲烷、正己烷、四氢呋喃、异辛烷、吡啶和甲苯）进行测定。结果：各残留溶剂组分均能被良好分离,各溶剂线性关系良好,精密度 RSD 均不超过 3.50%,平均回收率为 96.0%~105.0%。结论：本文建立的方法可用于达比加群酯中残留溶剂的测定。     

2种测定抗菌药物水分方法的比较研究

目的 采用气相色谱法和费休氏法测定抗菌药物中水分的含量,探讨使用气相色谱法测定抗菌药物水分含量的可行性。方法 气相色谱法采用顶空毛细管气相色谱-热导检测器法进行测定,使用Agilent HP-PLOT/Q毛细管色谱柱（30 m×0.530 mm×40 μm）,载气为高纯氦气,流量3 mL·min^-1,进样量250 μL,分流比20：1,进样口温度为200℃;柱升温程序：初始温度150℃,保持6 min,以60℃·min^-1的速率升到250℃,保持5 min;热导检测器温度为250℃,电流为70 mA。费休氏法采用中国药典2015年版四部通则0832中水分测定第一法中的容量滴定法。结果 除了注射用头孢曲松钠和注射用头孢唑肟钠外,其他抗菌药物样品2种测定方法测定结果无显著性差异。结论 本研究所建立的气相色谱法,可用于部分抗菌药物水分含量的测定。     

顶空-气相色谱法测定穿心莲内酯中有机溶剂残留量

目的：建立穿心莲内酯中有机溶剂残留量顶空毛细管气相色谱法测定方法.方法：色谱柱为CP-624毛细管柱（30m×0.32 mm×1.8μm）,N,N-二甲基甲酰胺为溶解介质,FID检测器.气化室温度200℃,检测器温度300℃,载气为氮气.柱温采取程序升温：起始温度为60 ℃,保持10min,以50℃·min^-1的速率升温至210℃,保持6 min.结果：穿心莲内酯中乙醇内酮及三氯甲烷得到完全分离,3批样品测定结果符合规定.结论：该方法简单、灵敏、准确.     

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.