顶空气相色谱法测定几丁糖酯中溶剂残留

目的 :建立顶空气相色谱法分析几丁糖酯中溶剂残留。方法 :采用水溶液顶空和固体顶空 2种气相色谱法 ,用AC -2 0石英毛细管色谱柱 ,以正丙醇为内标进行定量。结果 :水溶液顶空气相色谱法乙醇的线性范围为 8～ 192 μg·mL-1,丙酮的线性范围为 2～ 6 4μg·mL-1;方法的回收率为乙醇 10 3 3% ,丙酮 95 71% ,RSD均为 4 2 % ;最低检测限溶液中乙醇为 4μg·mL-1,丙酮为 1μg·mL-1。固体顶空气相色谱法乙醇的线性范围为 0 16～ 2 4μg·mL-1,丙酮的线性范围为 0 16～ 1 6 μg·mL-1;方法的回收率为乙醇 96 32 % ,丙酮 10 2 1% ,RSD分别为 3 5 %和 2 6 % ;最低检测限乙醇为 0 12 μg·g-1,丙酮为 0 0 6 μg·g-1。结论 :此 2种方法简单 ,准确 ,灵敏度高 ,经显著性检验二者无显著性差异。     

高效液相色谱法测定克林沙星血药浓度

目的 :建立用高效液相色谱法测定血浆中克林沙星浓度的方法。方法 :血浆样品在酸性条件下 ,以Oasis小柱提取环丙沙星为内标 ,采用LichrosorbC18(5 μm)柱 ,流动相为乙腈 - 0 0 5mol·L-1柠檬酸三乙胺溶液 (pH 2 5 ) (2 0∶80 ) ,流速为 1 0mL·min-1,检测波长 30 0nm ,克林沙星和内标的保留时间分别为 7 1min和 4 5min。结果 :线性范围在 0 0 3～10 μg·mL-1(r=0 9998) ,最低检测浓度为 0 0 2 μg·mL-1,RSD <7%。用本法测定了 6只大鼠灌胃剂量 5 0mg·kg-1克林沙星后血浆中克林沙星的浓度经时变化过程。结论 :本方法可用于克林沙星的血药浓度测定及药代动力学研究。     

HPLC法同时测定血浆地西泮及其代谢物浓度

目的 :建立同时测定血浆中地西泮及其代谢物浓度的方法。方法 :选用ZORBAXRP C18柱 (15 0mm× 4 6mm ,5 μm) ;甲醇 - 2 5mmol·L-1醋酸铵溶液 (6 0∶4 0 ,V/V)作流动相 ;流速 0 8mL·min-1;检测波长 2 30nm。取血浆样品 0 5mL ,在碱性条件下用二氯甲烷 -正己烷提取 ,HPLC检测。结果 :本法对替马西泮、去甲地西泮和地西泮 3种物质的最低检测限均为 2 μg·L-1,线性范围为 10～ 15 0 0 μg·L-1;奥沙西泮的最低检测限为 5 μg·L-1,线性范围为 2 0～ 15 0 0 μg·L-1。回收率均接近 10 0 % ,日内、日间RSD <5 %。结论 :本法能同时测定血浆中地西泮及其代谢物浓度 ,具有重现性好 ,灵敏、可靠 ,可用于地西泮中毒的监测     

RP-HPLC测定甘草酸单铵脂质体的含量及包封率

目的　建立甘草酸单铵脂质体含量及包封率的测定方法。方法　使用RP -HPLC ,YMC -PackODS -A柱 (S - 5 μm ,1 5 0mm× 6 .0mm) ,流动相为甲醇 -水 -四氢呋喃 - 5 %醋酸铵 (5∶9∶3∶4 ) ,流速 1ml·min-1 ,柱温为室温 ,检测波长 2 5 8nm ,用葡聚糖凝胶柱分离游离药物。结果　甘草酸单铵与辅料及溶剂峰分离良好 ,线性范围为 2 .5～ 2 5 μg·ml-1 (r=0 .9999,n =5 ) ,加样回收率在 99.4 %～ 1 0 0 .7%之间 ,RSD =2 .2 3%。结论　所用方法准确 ,可用于甘草酸单铵脂质体的含量及包封率测定     

反相离子对高效液相色谱法测定泰必治注射液A中4种组分的含量

目的 :采用反相离子对高效液相色谱法测定泰必治注射液A中盐酸利多卡因、地塞米松、卡巴芬乙酸 (钠盐 )与保泰松钠 4种组分的含量。方法 :采用YWG -C1 8(10 μm ,4 5mm× 15 0mm)色谱柱 ,以乙腈 -水 (4 5∶5 5 ,含 2 5mmol·L- 1十六烷基三甲基溴化铵 )为流动相 ,流速 1 5mL·min- 1 ,柱温 40℃ ,检测波长 2 30nm。结果 :本法可同时测定 4种组分的含量。盐酸利多卡因在 13～ 6 4μg·mL- 1 、地塞米松在 4 5～ 38μg·mL- 1 、卡巴芬乙酸 (钠盐 )在 2 6 9～ 16 14μg·mL- 1 、保泰松钠在 40 2～ 2 0 77μg·mL- 1 范围内 ,峰面积与其浓度呈良好的线性关系 ;平均回收率 (n =5 )依次为 99 9% (RSD =1 2 % ) ,10 1 0 % (RSD =0 4% ) ,10 0 5 % (RSD =0 2 % ) ,10 0 6 % (RSD =0 8% )。结论 :方法简便、快速、准确 ,可作为样品的检测方法。     

格拉司琼血药浓度的高效液相色谱分析

目的 :建立人血浆中格拉司琼浓度的反相高效液相色谱测定方法。方法 :液 液萃取法分离纯化血浆样品 ,采用荧光检测器 ,以甲醇 磷酸盐缓冲液 (pH 2 .2 ,0 .0 2mol·L- 1含 3 .0 %三乙胺 ) ( 6 3∶3 7)为流动相 ,色谱柱为Shim PackCLC ODS柱( 150mm× 6 .0mm) ,并阐述了血浆中格拉司琼色谱峰形变和分裂的可能机理。结果 :格拉司琼色谱峰对称、不拖尾 ,萃取回收率达 92 % ,空白血浆和代谢物不干扰测定 ,血药浓度线性范围为 0 .5～ 6 0 .0 μg·mL- 1(r =0 .9995) ,最低检测限 0 .3 μg·mL- 1,方法回收率为 98.43 %～ 10 0 .4% ,日内RSD 2 .3 %～ 3 .8% ,日间RSD 2 .9%～ 4.6 %。结论 :此法简便、准确 ,灵敏度高 ,选择性好。     

HPLC／MS测定人血浆中盐酸班布特罗及其代谢物特布他林的浓度

目的 :用高效液相 /质谱联用法测定人血浆中盐酸班布特罗及其代谢物特布他林的浓度。方法 :液相 :采用SupelcodiscoveryC18色谱柱 (5 μm ,2 5 0mm× 4 6mm) ;柱温 40℃ ;流动相为甲醇 -醋酸铵溶液 (0 0 0 7mol·L-1) (2 0∶80 ) (并用冰醋酸调 pH =4 8) ,流速 0 6mL·min-1,进样量 6 0 μL ;质谱 :大气压化学电离源 (APCI) ,选择性监测 (SIR)质荷比 (m/z)分别为 2 2 6 (特布他林 ) ,2 6 0 (内标 ) ,36 8(班布特罗 )带正电荷的分子离子峰定量。样品用固相萃取小柱提取处理。结果 :班布特罗线性范围 0 12 5～ 16 μg·L-1,最低检测浓度为 0 0 5 μg·L-1。特布他林线性范围 0 312 5～ 40 μg·L-1,最低检测浓度为 0 0 5 μg·L-1。班布特罗和特布他林的萃取回收率均在 90 %以上 ,日内、日间的RSD皆小于 15 %。结论 :适用于临床上测定血浆中盐酸班布特罗及其代谢物特布他林的浓度及药动学的研究     

高效液相色谱法测定米非司酮的血药浓度

目的　建立测定米非司酮血药浓度的方法。方法　以乙腈∶水 (70∶3 0 )为流动相 ,炔诺酮作内标 ,血浆样品经用乙醚萃取后上样 ,经C18柱分离后 ,在紫外波长 3 0 2nm处检测米非司酮 ,在 2 40nm处检测炔诺酮。结果　线性范围 0 .0 5～ 10 .0 μg·mL-1(r =0 .9995 )。平均相对回收率在 95 %～ 110 %之间 ,日内和日间RSD均小于 6%。米非司酮最低检出限为 0 .0 1μg·mL-1,萃取回收率大于 90 %。结论　本法快速、简便、准确、灵敏 ,可用于米非司酮的药物动力学研究     

HPLC法快速测定5—氟尿嘧啶血药浓度

目的 :建立反相高效液相色谱法测定人血清中 5 -氟尿嘧啶浓度。方法 :血清样品用乙酸乙酯提取 ,水浴氮气吹干 ,残留物用水溶解后进样。色谱柱为C1 8柱 (2 5 0mm× 4 6mm) ,水为流动相 ,流速 1 0mL·min- 1 ,紫外检测波长 2 73nm ,桂皮酸为内标。结果 :本法最低检测浓度为 0 0 5 μg·mL- 1 ,线性范围为 1 0～ 5 0 0 μg·mL- 1 ,日内RSD为 2 7%～ 4 1% ,日间RSD为 3 8%～ 4 7(n =4)。结论 :该法适用于 5 -氟尿嘧啶的药代动力学研究及临床血药浓度检测。试验结果表明 ,该方法经济、简便、快速、灵敏度高、重现性好。     

反相高效液相色谱法测定兔血浆中醋酸诺美孕酮的浓度

目的 :建立反相高效液相色谱法测定血浆中醋酸诺美孕酮的浓度。方法 :血浆样品用乙醚提取 ,选用WatersμBondapakC18(30 0mm× 3 9mm ,10 μm)为分析柱 ,甲醇 -水 (70∶30 )为流动相 ,流速为 1 2mL·min-1,米非司酮为内标 ,检测波长为 30 0nm。结果 :醋酸诺美孕酮线性范围为 0 1～ 10 μg·mL-1,最低检测浓度为 6 0ng·mL-1(S/N =3)。样品平均方法回收率为 95 2 0 % ,日内、日间精密度的RSD均小于 5 %。结论 :此方法稳定、可靠 ,可用于醋酸诺美孕酮血药浓度分析及药代动力学研究。     

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.