HS-SPME-GC-MS分析怀牛膝不同炮制品中的挥发性成分

摘 要 目的：对怀牛膝生品、盐制品和酒制品中挥发性成分进行分析和比较。方法: 采用顶空固相微萃取法(HS SPME)分别萃取怀牛膝生品、盐制品和酒制品中挥发性成分,并用气相色谱 质谱(GC MS)联用技术对怀牛膝生品及其盐制品和酒制品中的挥发性成分进行分析鉴定,利用峰面积归一化法测定各成分相对百分含量。结果: 共鉴定出38种化合物,从怀牛膝生品、盐制品和酒制品中分别鉴定出23、16和15种化合物,分别占其挥发性成分总含量的79.14%、49.80%和44.57%,三者含有共同挥发性成分4种。与怀牛膝生品相比,盐制品中新增了10种化合物、减少了17种化合物,而酒制品中新增了9种化合物、减少了17种化合物。结论: 不同炮制方法对怀牛膝中化学成分的种类及含量有一定影响。采用HS SPME GC MS联用技术能快速有效地分析怀牛膝不同炮制品中的挥发性成分,为怀牛膝炮制品的质量评价及应用提供科学指导。     

天山假狼毒不同部位挥发性成分比较分析研究

摘 要 目的：用GC MS分析比较天山假狼毒叶、花和根中挥发性成分。方法: 采用索氏提取法提取天山假狼毒叶、花和根中的挥发性成分,经GC MS联用技术对挥发性成分进行分析鉴定, 采用色谱峰面积归一化法计算各挥发性成分的含量。结果:结果共鉴定出179个挥发性成分,其中天山假狼毒叶中81个,相对含量占总挥发性成分总量的82.77%;花中108个,相对含量占总挥发性成分总量的82.85%;根中112个,相对含量占总挥发性成分总量的85.98%;三者共同含有挥发性成分33个,共有成分在叶子中占总挥发性成分的39.24%,在花中占总挥发性成分的35.86%, 在根中占总挥发性成分的48.89%。其中（Z,Z） 9,12 十八碳二烯酸在天山假狼毒叶、花、根挥发性成分中相对含量都最高,分别为11.12%、9.8%、22.49%。结论:天山假狼毒叶、花、根挥发性成分接近,但在组分和含量上存在一定的差异。     

紫花地丁及其混用品挥发性成分比较

摘 要 目的：分析紫花地丁及其混用品苦地丁的挥发性成分差异,快速区别紫花地丁和苦地丁。方法: 采用固相微萃取(SPME)法萃取紫花地丁和混用品苦地丁中的挥发性成分,并运用气相色谱 质谱(GC MS)联用法对其挥发性成分进行分析。 结果: 共检测出62个成分,鉴定出了42个成分,主要为烯类、酮类和醛类。从紫花地丁中分离出43个峰,鉴定出了28个成分,占挥发油总量的66.93%;从其混用品苦地丁中分离出22个峰,鉴定出了17个成分,占挥发油总量的97.02%。结论: 紫花地丁及其混用品的挥发性成分总离子流图的峰型和化学成分差异都较大,两者的共有成分有3种,含量差异较大,紫花地丁的挥发性成分中含量最高的是2 戊酰呋喃(18.01%),其混用品苦地丁挥发性成分中含量最高的是1 石竹烯(46.06%)。本方法快速稳定,可用于区别紫花地丁和苦地丁。     

HS-SPME-GC-MS联用分析不同产地山柰挥发性成分

摘 要 目的：分析比较不同产地山柰的挥发性成分,为后续药理活性研究奠定物质基础。方法: 首次采用顶空固相微萃取 气相色谱质谱联用(HS SPME GC MS)技术分别对广西、广东及云南山柰中挥发性化学成分进行提取和分析鉴定,并利用面积归一化法计算各成分的质量分数。结果:共鉴定出42种化学成分,主要为萜类、烃类、酯类和芳香族化合物。从广西山柰挥发性物质中分离出41个色谱峰,鉴定出38种化学成分,占挥发性成分总量的99.78%;从广东山柰挥发性物质中分离出37个色谱峰,鉴定出26种化学成分,占挥发性成分总量的80.49%;从云南山柰挥发性物质中分离出31个色谱峰,鉴定出24种化学成分,占挥发性成分总量的64.72%。结论:广西、广东及云南山柰的挥发性成分总体差异不大,3个产地的特征性成分均为甲氧基肉桂酸乙酯、肉桂酸乙酯及十五烷,但3个成分的相对含量大不相同,广西山柰中三者的相对含量分别为45.02%、17.18%、9.08%;广东山柰中三者的相对含量分别为41.08%、16.25%、8.04%;云南山柰中三者的相对含量分别为30.78%、15.66%、7.89%。其中甲氧基肉桂酸乙酯为山柰的主要活性成分之一,由此可推断广西、广东山柰质量优于云南山柰。本试验同时为山柰的道地性提供了佐证,并为山柰的进一步开发提供参考依据。     

HS-SPME-GC-MS联用分析醋制南北五味子中挥发性成分

摘 要 目的：分析和比较醋制南北五味子挥发性成分。方法: 采用顶空固相微萃取法(HS SPME)萃取醋制南北五味子中挥发性成分,结合GC-MS法对其挥发性成分进行分析。 结果: 从醋制南五味子中鉴定出20种化学成分,从醋制北五味子中鉴定出21种化学成分,分别占各自挥发性成分总量的99.55%和99.90%。结论:醋制南北五味子的挥发性成分在种类和含量上差异较大,为快速鉴定醋制南北五味子提供科学依据。     

HS-SPME-GC-MS分析炮制前后苍耳子挥发性成分

摘 要 目的：分析苍耳子生品及炒制品中挥发性成分的化学成分及相对含量的变化。方法: 采用顶空固相微萃取法（HS-SPME）结合气相色谱 质谱（GC MS）联用技术对苍耳子的生品及炒制品挥发性成分进行分析;以峰面积归一化法计算各组分的相对百分含量。结果: 从苍耳子生品和炒制品中分别分离鉴定出26种和27种化合物,共有成分19种,分别占挥发性成分总量的68.69%和90.08%,其中生品含量较高的成分有桉叶油醇(15.3%)、樟脑（9.6%）、冰片（6.89%）等,炒制品中成分含量较高的成分有薄荷醇（24.09%）、冰片（18.48%）、桉叶油醇(7.19%)等。结论:炒制品中薄荷醇、冰片等具有治疗鼻炎作用的相对含量较生品有明显提高,采用HS-SPME GC MS联用技术分析苍耳子生品及炒制品中挥发性成分及相对含量变化,可以从挥发性成分的变化方面为苍耳子生品及炒制品的功效差异的物质基础奠定一定的理论基础,为其进一步研究和综合利用提供科学依据。     

反相离子对高效液相色谱波长切换法测定复方苦参水杨酸散中4个成分的含量

摘 要 目的：采用反相离子对高效液相色谱结合波长切换技术,测定复方苦参水杨酸散中苦参碱,氧化苦参碱,水杨酸,苯甲酸等4个成分的含量。方法: 采用Agilent ZORBAX SB C18色谱柱（150 mm×4.6 mm,5 μm）,以乙腈 0.1%磷酸溶液（16∶84）（每100 ml中加庚烷磺酸钠0.2 g）为流动相,流速：1.0 ml·min^-1;检测波长：0~12 min,220 nm;12~25 min,280 nm;柱温30 ℃;进样量10 μl。结果: 苦参碱,氧化苦参碱,水杨酸,苯甲酸的线性范围分别是0.006 030～0.120 6 μg（r=0.999 4）,0.016 56～0.331 2 μg（r=0.999 9）,0.717 1～14.34 μg（r=0.999 9）,0.512 0～10.24 μg（r=0.999 9）;平均加样回收率分别为98.14%,97.20%,97.05%,98.39%,RSD分别为1.38%,0.32%,0.81%,1.26%（n=6）。结论:该方法快速,准确,可用于复方苦参水杨酸散中苦参碱,氧化苦参碱,水杨酸,苯甲酸等4个成分的含量测定。     

藿香祛暑软胶囊GC特征图谱研究及2种成分的含量测定

摘 要 目的：建立藿香祛暑软胶囊的GC特征图谱,同时测定丁香酚和百秋李醇的含量。 方法: 采用GC分析方法,HP 5毛细管柱（30 m×0.32 mm,0.25 μm）,FID检测器。进样口温度：250℃,检测器温度：280℃,分流进样。程序升温：初温80℃,以6℃·min-1速度升至160℃,保持3 min,以10℃·min-1速度升至210℃,保持20 min,载气为氮气,载气流速：1.2 ml·min-1。 结果: 特征图谱共有9个特征峰,18批样品与对照图谱相似度均在0.90以上,丁香酚和百秋李醇分别在15.586～779.315 μg·ml-1（r=0.999 9）和17.736～886.800 μg·ml-1（r=0.999 8）范围内线性关系良好,平均加样回收率分别为101.46%,104.02%,RSD分别为1.87%,2.33%（n=6）。 结论: 该方法简单,快速,准确,重复性好,GC特征图谱结合2成分含量测定可用于藿香祛暑软胶囊中挥发性成分的质量控制。     

固相微萃取-气质联用法分析浅裂鳞毛蕨挥发性成分

摘 要 目的： 研究浅裂鳞毛蕨的挥发性成分。方法: 采用气相色谱 质谱联用技术首次对浅裂鳞毛蕨的挥发性成分进行分析和鉴定。结果: 从浅裂鳞毛蕨根中鉴定了28个化合物,占根中挥发性成分的86.84%,从叶中鉴定了24个化合物,占叶中挥发性成分的82.79%。结论: 正壬醛有可能是浅裂鳞毛蕨叶中的主要香气成分,丁羟基甲苯和石竹烯有可能是浅裂鳞毛蕨中的药效成分。     

双波长HPLC法同时测定复方肤清洗剂中3种指标性成分含量

摘 要 目的：建立双波长HPLC法同时测定复方肤清洗剂中绿原酸、咖啡酸、芍药苷3种指标性成分含量的方法。方法: 采用Inertsil C18柱（250 mm×4.6 mm,5 μm）为色谱柱,柱温40℃,以乙腈-0.02%磷酸水溶液（17∶83）为流动相,流速为1.0 ml·min^-1,检测波长分别为323 nm、230 nm。结果:绿原酸、咖啡酸和芍药苷分别在7.50~120.00 μg·mL^-1,2.50~40.00 μg·mL^-1,14.06~225.00 μg·mL^-1范围内线性关系良好,r分别为0.999 9,0.999 8,0.999 7;平均加样回收率分别为98.55%,94.52%,99.18%,RSD分别为1.66%,0.98%,0.65%（n=6）。结论:该方法简便快捷、结果准确、专属性强,可用于复方肤清洗剂的质量分析与控制。     

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.