高效液相色谱法测定替加氟片的含量和溶出度

目的 建立测定替加氟片含量及其溶出度的高效液相色谱法.方法 分析柱为惠普C18柱(250 mm×4.6mm,5μm),流动相为甲醇-乙腈-水(10:5:85),流速为1.0 mL/min,检测波长为271 nm.结果 替加氟进样量在2.041-4 082 ng范围内与峰面积线性关系良好(r=0.999 9),平均回收率为99.56%,RSD=0.13%(n=9).替加氟的检测限和定量限分别为1.4 ng和4.7 ng.结论 所用方法简便、可靠、准确,可用于替加氟片的常规分析.     

HPLC法测定不同厂家注射用盐酸头孢替安的含量

目的:运用HPLC法测定不同厂家注射用盐酸头孢替安的含量。方法:采用高效液相色谱法,色谱条件:Spherisorb C18色谱柱(150 mm×4.6 mm,5μm),流动相为磷酸盐缓冲液-乙腈(88∶12),检测波长为254 nm,流速为1.0 ml/min,柱温为25℃,进样量10μl。结果:头孢替安在0.39mg/ml~2.72 mg/ml浓度范围内线性关系良好(r=0.9999),平均加样回收率为99.61%(RSD=1.10%)。结论:该方法快捷、可靠、灵敏度高,可用于注射用盐酸头孢替安的含量测定。     

RP-HPLC法测定注射用磷酸氟达拉滨中磷酸氟达拉滨的含量

目的建立以反相高效液相色谱法测定注射用磷酸氟达拉滨中磷酸氟达拉滨含量的方法。方法色谱柱为AgilnetXDB-C18(150mm×4.6mm,5μm),流动相为0.008mol/L磷酸二氢钾溶液:乙腈=95:5,流速为1.0=ml/min,柱温为30℃,检测波长为261nm。结果磷酸氟达拉滨浓度在5～100μg/ml范围内与峰面积积分值呈良好线性关系(r=0.9997);平均回收率为99.6%,RSD=0.3%(n=9)。结论本方法操作简便,测定结果准确、重现性好,可用于测定注射用磷酸氟达拉滨中磷酸氟达拉滨的含量。     

椒葛软胶囊中葛根素的含量测定

目的:建立椒葛软胶囊中葛根素含量测定的方法.方法:采用高效液相色谱法,色谱柱为HypersilODS柱(250mm×4.6mm,2.5μm).流动相为CH3OH-CHCl3-1.5%冰醋酸(22:1:77),波长为250nm.结果:葛根素的线性范围为0.042～0.210mg·mL,r=0.999 9;平均加样回收率为100.4%,RSD为1.17%.结论:用高效液相色谱法测定椒葛软胶囊中的葛根素含量,方法准确、简便易行.     

高效液相色谱法测定三氟甘露糖的含量

目的:建立高效液相色谱法测定三氟甘露糖的含量.方法:采用ODS C18-Ultrasphere色谱柱(250 mm×4.6 mm,5 μm),以水-乙腈(35:65)为流动相,流速1.0 mL/min,检测波长220 nn,柱温30℃.结果:三氟甘露糖在0.25～2.0 mg/mL浓度范围内峰面积与浓度线性关系良好(r=0.998 9),方法的平均回收率为99.2%(RSD为0.87%).结论:高效液相色谱法可用于三氟甘露糖含量测定.     

HPLC法测定替吉奥片中3种成分的含量

建立高效液相色谱法测定替吉奥片中奥替拉西钾、吉美拉西以及替加氟的含量。采用KromasilC18色谱柱;流动相:磷酸二氢钾缓冲溶液(取磷酸二氢钾1.36g,加水800mL与三乙胺10mL,用磷酸调pH至4.5)-甲醇(85∶15),流速:1.0mL·min-1,检测波长:266nm,进样量:10μL,柱温:室温。奥替拉西钾、吉美拉西和替加氟分别在0.17～2.82μg(r=0.9993),0.06～0.81μg(r=0.9996),0.16～2.88μg(r=0.9998)范围内线性良好。平均回收率分别为99.8%(RSD=0.31%),99.7%(RSD=0.73%),99.9%(RSD=0.38%)。该方法简单、灵敏、准确、专属性强,可用于替吉奥片的质量控制。     

替加氟温敏凝胶含量测定方法的建立

目的:建立以高效液相色谱法测定替加氟温敏凝胶含量的最佳方法。方法:通过对中国药典和参考文献中测定替加氟温敏凝胶含量的HPLC方法进行比较,并根据凝胶剂特点考察检测条件、样品处理方法,测定替加氟温敏凝胶含量,对各方法回收率进行考察,做出综合评价。 结果:在流动相为:0.02 mol·L^-1磷酸二氢钾溶液-甲醇(60:40)的条件下,替加氟在2~15 μg·ml^-1范围内线性关系良好(r=0.999 8),平均加样回收率为99.71%,精密度RSD低于2%,符合要求。3批样品中替加氟的平均含量为标示量的(99.90±0.78)%。结论:本检测方法简便、快速、结果准确、重复性好,可为替加氟温敏凝胶的质量控制提供分析依据。     

注射用赖氨匹林的两种含量测定方法

目的:采用高效液相色谱法和紫外分光光度法同时测定注射用赖氨匹林的含量,为质量控制提供有效的分析手段.方法:高效液相色谱法:Hypersil C18(1500mm×4.6mm,10μm),以甲醇-0.1%三乙胺溶液(1:1.冰醋酸调节pH至3.5)为流动相,检测波长为280nm,按外标法以峰面积计算.紫外分光光度法:检测波长210nm.结果:高效液相色谱法:阿司匹林和水杨酸在60.34～905.10μg/ml和1.20～18.00μg/ml浓度范围内呈良好的线性关系,其线性相关系数分别为0.9999和0.9999;加样回收率分别为98.76%～99.29%(RSD=0.59%～0.93%)和98.49%～99.69%(RSD=0.80%～1.01%).紫外分光光度法:赖氨匹林浓度在4.0～14.0μg/ml范围内与吸收度有良好的线性关系,回归方程为:Y=0.0548X-0.0299,r=0.9998,方法平均回收率为99 8%～100.7%,RSD为1.62%～1.81%.结论:两种方法均可用作注射用赖氨匹林的质量控制.     

高效液相色谱法测定注射用左卡尼汀的含量

目的:建立高效液相色谱法测定注射用左卡尼汀的含量。方法:色谱柱为C18柱(150mm×4.6mm,5μm),以庚烷磺酸钠-磷酸盐缓冲液-甲醇(555mg∶950mL∶50mL)为流动相,检测波长为225nm,流速为1mL.min-1。结果:左卡尼汀在5.1~30μg范围内呈良好的线性关系(r=0.9998),平均回收率为99.46%,RSD为0.69%。结论:本方法精密可靠,可作为注射用左卡尼汀质量控制的方法。     

高效液相色谱法测定注射用奥拉西坦的含量

目的建立测定注射用奥拉西坦含量的高效液相色谱法。方法色谱柱为Ultimate C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-水(5∶95),检测波长为214 nm,流速为0.8 mL/min。结果奥拉西坦含量测定线性范围为0.040 4～0.323 2 g/L(r=0.999 8),平均回收率为99.6%,RSD为1.1%(n=6)。结论该含量测定方法简便、准确、重复性好,可有效控制注射用奥拉西坦的质量。     

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.     

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.     

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.