厚朴的气相色谱—质谱分析

尊文用ＨＰ－５毛细管气－质联用法分析了厚朴药材的化学成分。色谱柱为ＨＰ－５柱（３０ｍ×０．２５ｍｍ）；程序升温１５０℃６℃／ｍｉｎ，２２０℃（１５ｍｉｎ）；进样口及检测器度均为２８０℃；流速１．０ｍｌ／ｍｉｎ，分流比１：３０。质谱条件：电子轰击源（Ｅｌ）；电离温度：１７８℃；电子能量：７０ｅＶ。除了确证含有β－桉油醇、厚朴酸及和厚朴酚外，还发现可能含有δ－蛇床烯、十六酸、（Ｚ，Ｚ）－９，１２－十八     

反相HPIC法测定血清布洛芬含量

本文以消炎痛为内标，用反相ＨＰＩＣ测定血清中的布洛芬。色谱柱为ＹＷＧＣ（１８）（１０μｍ）２００ｍｍ×５ｍｍ。流动相为甲醇－２０ｍｍｏｌ／Ｌ。磷酸二氢钾缓冲液（７０：３０，ｐＨ３．８）。流速为１ｍｌ／ｍｉｎ。检测波长为２２５ｎｍ。色谱柱柱温为５０℃。布洛芬和内标的保留时间分别为７．２和５．２ｍｉｎ。布洛芬的检测限为２ｎｇ（Ｓ／Ｎ≥４：１）。血清样品的预处理采用１：１的乙腈沉淀蛋白后直接进样。血清布洛芬浓度在０．５～６４μｇ／ｍｌ范围呈线性关系（ｒ＝０．９９９６）。天内天间精密度分别为１．６％～３．９％和２．１％～５．０％。     

HPLC法测定泻痢停片中磺胺甲噁唑和甲氧苄氨嘧啶的含量

用ＨＰＬＣ法测定泻痢停片中磺胺甲恶唑和甲氧苄氨嘧啶的含量。色谱柱为Ｃ１８柱,流动相为０．０５ｍｏｌ／ＬＫＨ２ＰＯ４－０．０５ｍｏｌ／ＬＮａ２ＨＰＯ４－甲醇（２２：２：１５）,流速为１．２ｍｌ／ｍｉｎ,检测波长为２４０ｎｍ。磺胺甲恶唑在２０～６０ｕｇ／ｍｌ范围内线性良好。平均回顾率为１００．４％（ＲＳＤ＝０．４１％）;甲氧苄氨嘧啶在４～１２ｕｇ／ｍｌ范围内线性良好,平均回收率为９９．４％（ＲＳＤ＝０     

银杏和苦荞麦制品中芦丁的RP—HPLC测定

采用ＲＰ－ＨＰＬＣ法测定了银杏和苦荞制品中芦丁的含量，以十八烷基硅烷键合硅胶为填料，柱温３５℃甲醇－３６％醋酸－水（３９：２．３：５８．７）和甲醇－乙腈－３６％醋酸－水（２２：１０：２．６：６５．４）为流动相，１ｍｌ／ｍｉｎ，检测波长３５８ｎｍ，芦丁色谱峰形对称，分离度好，所测苦荞麦快餐营养粉和天银口服液中芦丁含量分别为０．０６９０％和０．０１６８％。     

银杏和苦荞麦制品中芦丁的RP－HPLC测定

采用ＲＰ－ＨＰＬＣ法测定了银杏和苦荞麦制品中芦丁的含量。以十八烷基硅烷键合硅胶为填料，柱温３５℃；甲醇－３６％醋酸－水（３９：２．３：５８．７）和甲醇－乙腈－３６％醋酸－水（２２：１０：２．６：６５．４）为流动相，１ｍｌ／ｍｉｎ；检测波长３５８ｎｍ，芦丁色谱峰峰形对称、分离度好。所测苦荞麦快餐营养粉和天银口服液　中芦丁含量分别为０．０６９０％和０．０１６８％。     

测定人血浆中吗啡浓度的GC—MS法及其在药代动力学研究中…

本文建立了测定血浆中吗啡浓度的气相色谱－质谱联用检测法，以纳洛酚做为内标物，吗啡和内标分离良好，保留时间分别为：吗啡４．８ｍｉｎ，内标６．２ｍｉｎ。吗啡的相对回收率为７９－８３％，日内精密度为１．４０－２．２６％，日间精密度为０．５９－１．８４％，最低检测浓度为２ｎｇ／ｍｌ。     

呱西替柳胶囊及其相关物质的气相色谱法测定

用气相色谱法测定了胶囊剂中呱西替柳及有关物质的含量，色谱条件为：１．５％ＯＶ－１７固定液，进样口温度２４０℃，柱温２２０℃，ＦＩＤ检测器，气体流速：Ｎ２６０ｍＬ／ｍｉｎ，Ｈ２５０ｍＬ／ｍｉｎ，空气６００ｍＬ／ｍｉｎ，量程：１０＾２，衰减２＾６，纸速１ｍｍ／ｍｉｎ。呱西替测定以扑尔敏为内标物，主要杂质测定用外标法。     

毛细管气相色谱测定人血浆中5—单硝基异山梨醇酯

目的：建立测定人血浆中５－单硝基异山得醇酯（ＩＳ－５－ＭＮ）浓度的气相色谱检测法，方法：分析柱为ＨＰ－５毛细管柱，进样口，色谱柱及检测温度分别为２１０，１６０及２００℃，检测器为＾６３Ｎｉ电子捕获检测器，采用乙酸乙酯萃取血浆中ＩＳ－５－ＭＮ及内标２，４－二硝基甲苯。结果：ＩＳ－５－ＭＮ血药浓度在１０－８００ｎｇ／ｍｌ范围内线性关系良好（ｒ＝０．９９９８）最低检测浓度为５ｎｇ／ｍｌ，日内及日间差异均     

高效液相色谱法测定人血浆依托泊苷浓度

目的：建立一种快速、灵敏的高效液相色谱法测定人血浆中依托泊苷（Ｖｐ－１６）浓度的方法。方法：以替尼泊苷（ＶＭ－２６）为内标,采用惠普１１００型高效液相色谱仪,以 ＨＰ Ｈｙｐｅｒｓｉｌ ＯＤＳ ｃｏｌｕｍｎ（１２５ ｍｉｎ×４ｍｍ,５μｍ）为分析柱,前加ＨＰ Ｌｉｃｒｏ－ｓｐｈｅｒｅ保护柱;流动相为甲醇∶水＝４８∶５２（ｖ／ｖ）,流速为１．５ ｍｌ／ｍｉｎ;检测波长为２２０ｎｍ;室温２５℃。血浆样品经甲醇沉淀蛋白等处理后进样。结果;色谱峰分离良好,无干扰。线性方程为Ｙ＝０．９９２１Ｘ＋０．０４８ ２４,ｒ＝１．０００;线性范围：０．ｌ～１０．００μｇ／ｍｌ;检测限：０．１μｇ／ｍｌ。利用本法检测了一例Ｖｐ－１６ ３００ｍｇ、氟脲嘧啶１ｇ、顺铂８０ｍｇ的化疗患者血样,合并用药及代谢产物均对Ｖｐ－１６色谱峰无干扰。结论：本法是一种可靠的、快速灵敏的检测血浆中Ｖｐ－１６ 浓度的方法,适用于含Ｖｐ－１６的化疗方案的监测及药物动力学的研究。     

肉桂油气相色谱与气质联用分析

建立肉桂油中桂皮醛的含量测定方法和鉴定挥发化学成分。方法：气相色谱法,３ｍｍ＊４ｍ不锈钢柱,１０％ＰＥＧ－２０Ｍ为固定液,ＣｈｒｏｍｏｓｏｒｂＷＡＷ６０－８０目检测器,柱温１９０℃;气质联用,以ＨＰ－５毛细管柱,柱温起始１２０℃保持５ｍｉｎ后５℃．ｍｉｎ＾－１升温至１５０℃保持７ｍｉｎ,检测质荷比范围１０－４２５。结果桂皮醛在２－１０ｍｇ．ｍＬ＾－１范围内具良好线性关系,平均回收率为９８．３％－１     

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.