GC法测定丙酮酸乙酯的含量

摘 要 目的：建立测定丙酮酸乙酯原料含量的气相色谱法。方法: 色谱柱：Varian CP7502毛细管柱（25 m×0.25 mm,0.25 μm）;载气：氮气,流量为30 ml·min^-1;燃气：氢气,流量为40 ml·min^-1;助燃气：空气,流量为400 ml·min^-1;检测器：氢火焰离子化检测器（FID）;进样口温度：210 ℃;升温程序：初始温度为 40 ℃,以 15 ℃·min^-1的速度升至200 ℃;分流比：100∶1;进样量：1 μl。结果: 丙酮酸乙酯进样浓度在0.025 6~8.192 8 mg·mL^-1范围内与内标物的峰面积比值呈良好的线性关系（r=0.999 8）,平均加样回收率为99.99%,RSD为1.38%（n=9）。结论:建立的GC法准确、简便、快速、稳定性好,检测灵敏度高,适用于丙酮酸乙酯原料药的含量测定。     

GC法测定阿魏酸哌嗪中的残留溶剂

摘 要 目的：建立阿魏酸哌嗪中苯、氯乙醇与吡啶等残留溶剂的测定方法。 方法: 采用GC法,以DB 624（30 m×0.53 mm, 1.0 μm）弹性石英毛细管柱为色谱柱,载气为氮气,采用氢火焰离子化检测器;起始温度为50℃,维持5 min,以10℃·min^-1的速率升温至80℃,再以50℃·min^-1的速率升温至200℃,维持4 min;进样口温度为200℃,检测器温度为220℃;分流比为1∶1;进样量为1 μl;柱流速为3 ml·min^-1。结果: 苯在0.16～0.96 μg·mL^-1的浓度范围内线性关系良好（r=0.999 5）,平均回收率为95.7%（RSD=2.1,n=9）,检测限为0.16 ng;氯乙醇在16.11～96.65 μg·mL^-1的浓度范围内线性关系良好（r=0.999 7）,平均回收率为97.8%（RSD=2.1,n=9）,检测限为0.62 ng;吡啶在15.87～95.23 μg·mL^-1的浓度范围内线性关系良好（r=0.999 8）,平均回收率为99.2%（RSD=1.3,n=9）,检测限为0.15 ng。结论:本测定方法可靠、简便、结果准确、稳定性好,适用于本品残留溶剂的测定。     

顶空气相色谱法测定盐酸厄洛替尼中有机溶剂残留量

摘 要 目的：建立顶空毛细管气相色谱法测定盐酸厄洛替尼中有机溶剂残留量的方法。方法: 采用顶空毛细管气相色谱法,色谱柱为DB 624毛细管柱（30 m×0.53 mm,3.0 μm）,载气为氮气,流速为2.0 ml·min^-1,进样口温度为190 ℃,FID检测器温度为230 ℃,采用程序升温：初始温度为35 ℃,保持8 min,以28 ℃·min^-1升温至170 ℃,保持8 min,再以32 ℃·min^-1升温至200 ℃,保持7 min。顶空瓶平衡温度为100 ℃,时间30 min。结果: 乙醇、异丙醇、二氯甲烷、正丁醇分别在0.68~409.14 μg·mL^-1（r=0.999 8）、0.67~404.88 μg·mL^-1（r=0.999 8）、1.71~51.31 μg·mL^-1（r=0.999 7）、0.72~431.12 μg·mL^-1（r=0.999 8）浓度范围内线性关系良好,平均回收率分别为99.0%（RSD=0.41%,n=9）、100.2%（RSD=0.52%,n=9）、97.1%（RSD=1.75%,n=9）、102.5%（RSD=1.08%,n=9）。结论:该方法简便、准确性好,适用于盐酸厄洛替尼中4种有机溶剂残留量的测定。     

气相色谱法测定间甲酚的含量

摘 要 目的： 建立药用辅料间甲酚含量测定的气相色谱分析方法。方法: 采用气相色谱法,色谱柱：Agilent DB 225 MS（30 m×0.25 mm,0.25 μm）;升温程序：起始温度为90℃,维持10 min,以每分钟2℃的速率升至120℃,再以每分钟10℃速率升至150℃,维持5 min,进样口温度为200℃,检测器为火焰离子化检测器,温度为250℃。流速为1.8ml·min^-1;分流比为1∶30;载气为氮气。结果: 间甲酚在0.6～1.8 mg·ml^-1的范围内,其浓度与样品和内标峰面积的比值呈良好线性关系;平均回收率为96.0%,RSD为2.6%（n=9）。三批样品的测量结果分别为99.3%、98.7%和98.4%。结论:所建立的气相色谱法专属性强,准确度高、重复性好,可用于间甲酚的质量控制。     

GC-MS法测定奥拉西坦原料中的潜在遗传毒性杂质

摘 要 目的：建立同时测定奥拉西坦原料药中潜在遗传毒性杂质氯乙酸甲酯和(R,S)4 氯 3 羟基丁酸乙酯的方法。方法: 采用GC-MS法,使用乙酸乙酯进行提取。色谱柱为VF 1701 ms毛细管柱（30 m×0.25 mm,0.25 μm）,柱温采用程序升温,进样口温度为220℃,柱流量为1.0 ml·min^-1,吹扫流量为5.0 ml·min^-1,进样方式为分流进样,分流比为5∶1,载气为高纯氦气,检测器为MS检测器,离子源温度为230℃,接口温度为230℃,溶剂延迟时间为4 min,离子化模式为电子轰击离子化模式,扫描（检测）方式为选择性离子检测,电子能量为70 eV,进样量为1.0 μl。结果:2种杂质成分之间的分离度符合要求,浓度线性范围均为50～400 ng·mL^-1（r≥0.999 5）,加样回收率分别为89.7%～96.3%（RSD=2.3%,n=9）、91.0%～105.3%（RSD=4.4%,n=9）。结论:该方法简便、准确、灵敏、迅速,可用于奥拉西坦原料药中2种潜在遗传毒性杂质的测定。     

GC测定香砂平胃丸中苍术素、厚朴酚、和厚朴酚的含量

摘 要 目的： 建立香砂平胃丸中苍术素、厚朴酚、和厚朴酚的气相色谱含量测定方法。方法: ：采用HP-5毛细管柱（30 m×0.32 mm×0.25μm）,以氮气为载气,流速为2.0 ml·min^-1,进样口温度为300℃,检测器(FID)温度为300℃,进样量为1 μl,分流比为20∶1;采用程序升温模式,起始温度为100℃,保持7 min,以20℃·min^-1的速率升温至250℃,保持10 min。结果: 苍术素、厚朴酚、和厚朴酚分别在4.264～85.280 μg·ml^-1（r=0.999 7）、9.856～197.120 μg·ml^-1（r=0.999 5）、10.040～200.800 μg·ml^-1（r=0.999 6）范围内线性关系良好,平均回收率分别为98.2%、98.6%、99.3%,RSD分别为1.5%、1.5%、1.9%（n=6）。结论:该方法简便、准确、可靠,可用于香砂平胃丸的质量控制。     

复方醋酸氟轻松酊中间苯二酚、冰片、甘油和二甲亚砜的含量测定

摘 要 目的：建立GC法测定复方醋酸氟轻松酊中二甲亚砜、间苯二酚、冰片和甘油的含量。方法: 色谱柱：HP INNOWax(30.0 m×0.32 mm,0.25 μm）;进样口温度：280℃;检测器温度：290℃;分流比：10∶1;以氮气为载气,流速：2.0 ml·min^-1 ;程序升温：初始温度100℃,保持5 min,以20℃·min^-1 的速率升温至240℃,保持8 min;氢气流量：35 ml·min^-1 ;空气流量：350 ml·min^-1 ;尾吹气流量：25 ml·min^-1 ;以奈为内标。结果: 二甲亚砜、间苯二酚、冰片和甘油的浓度分别在99.20～793.60 μg·ml^-1 (r=0.999 9)、507.25～4 058.00 μg·ml^-1 (r=0.999 9)、102.20～817.60 μg·ml^-1 (r=1.000 0)、316.20～2 529.60 μg·ml^-1 (r=1.000 0)范围内线性关系良好,平均回收率分别为98.58%、98.34%、98.19%、102.29%,RSD分别为3.80%、3.93%、2.87%、3.65%(n=9)。结论: 该方法简便、准确、可靠,可用于复方醋酸氟轻松酊中二甲亚砜、间苯二酚、冰片和甘油的质量控制。     

GC内标法测定盐酸美金刚分散片含量及含量均匀度

摘 要 目的：建立盐酸美金刚分散片含量及含量均匀度的GC测定法。方法: 样品用水溶解,氢氧化钠溶液碱化,二氯甲烷萃取。色谱系统采用HP 5气相色谱柱（50 m×0.32 mm,1.05 μm）;柱温为程序升温,起始温度为120℃,维持3 min,以10℃·min^-1的速率升温至220℃,维持7 min;采用氢火焰离子化检测器（FID）;分流比为1∶1;进样口温度为230℃;检测器温度为260℃;进样量为1 μl;载气为高纯氮;流速为3.0 ml·min^-1。以金刚烷为内标物,采用内标法以峰面积进行计算。 结果: 盐酸美金刚在0.05～1.0 mg·ml^-1浓度范围内和主成分与内标峰面积的比值呈良好的线性关系（r=0.999 7）;检测限和定量限分别为1.1 ng和3.3 ng;平均回收率为100.2%（RSD=0.73%,n=9）。结论:该方法操作简便,萃取过程毒性小,对环境污染小,且结果准确、精密度高、专属性强,可用于盐酸美金刚分散片含量及含量均匀度的测定。     

气相色谱法测定药用辅料苯甲醇的有关物质

摘 要 目的： 对药用辅料苯甲醇中有关物质检查方法进行研究。 方法: 采用气相色谱法,Agilent DB-wax毛细管柱（0.32 mm×30 m,1.8 μm）;柱温：起始温度50℃,以5℃·min^-1速率升温到220℃后,维持35 min;检测器为FID;进样口温度为200℃,检测器温度为310℃,并以气 质联用法对检测结果进行确证。结果: 各杂质在一定范围内峰面积与浓度呈良好的线性关系（r≥0.999 9）,平均回收率为96.1%～102.7%,定量限为1.37～3.63 ng。样品中检出杂质甲苯、氯化苄、苯甲醛、苄醚。结论: 本方法简便快捷、结果准确、方法可行,可用于药用辅料苯甲醇中有关物质的检测。     

百花定喘片质量标准的建立

摘 要 目的：建立百花定喘片中3种药材的薄层色谱（TLC）鉴别及薄荷脑的含量测定方法。方法: 采用TLC法对百花定喘片中的陈皮、麻黄、五味子进行定性鉴别;采用GC法对百花定喘片中的薄荷脑进行含量测定。色谱条件：采用DM 5（30 m×0.53 mm,1.5 μm）毛细管柱;进样口温度为200 ℃;FID检测器,检测器温度为300 ℃;柱温:初始温度为80℃,以8 ℃·min^-1的速率升至120 ℃,再以15 ℃·min^-1的速率升至185 ℃,保留10 min;载气为氮气,柱流量为3 ml·min^-1;进样量为1 μl,分流进样,进样分流比为1∶5。结果: 在TLC色谱中,3味药材均能得到很好的鉴别;薄荷脑在1.484～74.200μg·ml^-1浓度范围内与峰面积呈良好的线性关系(r=0.999 8) ,平均回收率为 97.76%,RSD= 0.58%（n=9）。结论: 该法专属性强,操作简单,重复性好,可用于百花定喘片的质量控制。     

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.