HPLC法测定刺五加提取物缓释微球中刺五加苷B的含量

目的:建立测定刺五加提取物缓释微球中刺五加苷B含量的方法.方法:采用HPLC法.色谱柱为Agilent Eclipse Plus C18(250 mm×4.6 mm,5 μm),流动相为乙腈:水(17:83),流速为1.0 ml·min-1,柱温为30℃,检测波长为220 nm,进样量为20 μl.结果:刺五加苷B浓度在10.00～120.00 μg·ml-1范围内线性关系良好(r=0.999 9);平均加样回收率为98.10%(RSD=0.98%,n=6).结论:该方法结果准确可靠,可以作为该制剂的质量控制方法.     

高效液相色谱法测定雷公藤类药材及其制剂中雷公藤甲素的含量

目的 建立雷公藤药材及其制剂中雷公藤甲素的HPLC测定方法.方法 外标法,色谱柱:Angilent ZORB-AXSC-C18(4.6 mm×25 cm,5 μm);流动相:甲醇-水(40∶60);检测波长:218 nm;柱温:25℃;流速:1.0mL·min-1;进样量:20 μL.结果 雷公藤甲素在0.049 8～0.249 0 mg·mL-1呈良好的线性关系,r=0.999 8(n=5),平均回收率为100.66%,RSD=1.60%(n=9).结论 本方法具有操作简便、准确,回收率好,精密度、重现性高,分析快速的优点.可作为雷公藤药材及其制剂中雷公藤甲素的定量分析和质量控制方法.     

卫生散的质量标准

目的:研究完善卫生散的质量标准.方法:薄层色谱法鉴别制剂中的红参、人工牛黄、五倍子;HPLC法测定制剂中没食子酸的含量,色谱柱为Waters C18(250 mm×4.6 mm,5 μm),流动相为甲醇-0.2%磷酸(8:92),流速为1.0 ml·min-1,检测波长为273 nm,柱温为30℃,进样量为10 μl.结果:鉴别阴性对照均无干扰;含量测定方法中没食子酸的线性范围为0.062 0～1.858 5 μg(r=0.999 9),回收率为101.8%(RSD=0.46%,n=6).结论:所建方法简单、可靠,可作为卫生散的质量控制标准.     

高效液相色谱法测定接骨七厘片中阿魏酸的含量

目的 建立接骨七厘片中阿魏酸的含量测定方法.方法 采用HPLC法,shimpack vp-ODS色谱柱(4.6mm×250 mm,5 μm);流动相:甲醇-水-磷酸(48∶52∶0.2);检测波长:274 nm;流速:1.0 mL·min-1.结果 峰面积对进样量的回归方程为Y=1.635×106X 2.517×102,r=0.999 9(n=5),阿魏酸的进样量在0.096～0.48 μg线性关系良好,平均加样回收率为98.59%(n=5),RSD=1.05%.结论 该方法简便可行,准确可靠.     

八角茴香中莽草酸的含量测定

目的建立八角茴香中莽草酸含量的测定方法.方法色谱柱为PHENOMENEX-ODS(250 mm×4.6 mm,5 μm);流动相为乙腈-水(2080),四丁基氢氧化铵6.6 mmol·L-1(2%磷酸调至pH 7.5);检测波长为223 nm;流速1.0 mL·min-1.结果莽草酸在0.498～8.972 μg范围内,峰面积与进样量呈良好的线性关系(r=0.999 0,n=3),平均加样回收率为97.91%～100.94%(RSD为1.32%～2.82%,n=3).结论本方法简便、准确、重复性好,可作为工业生产的质量控制标准.     

HPLC测定注射用头孢曲松钠舒巴坦钠的含量

目的 建立测定注射用头孢曲松钠舒巴坦钠含量的方法.方法 采用HPLC法,色谱柱为Alltech Alltima C18(250 mm×4.6 mm,5 μm);柱温30℃;流动相为5 mmol·L-1四丁基氢氧化铵的磷酸二氢钾溶液(30 mmol·L-1)-乙腈(90:10)(用磷酸调pH3.8);流速1.0 ml·min-1;检测波长220 nm;进样20 μl.结果 头孢曲松的线性范围为0.08～0.50 mg·ml-1(r=0.9999),平均回收率为99.4%;舒巴坦的线性范围为0.05～0.33 mg·ml-1(r=0.9999),平均回收率为99.6%(n=6).结论 所建方法简便、快速,准确可靠,可作为本制剂质量控制的方法.     

HPLC法测定小儿惊风散中甘草苷的含量

目的 建立小儿惊风散中甘草苷的测定方法,以控制制剂的质量.方法 采用高效液相色谱(HPLC)法测定小儿惊风散中甘草苷的含量.色谱柱为SSWAKOSILC18AR柱(5 μm,4.6 mm×250 mm);流动相:乙腈-甲醇-0.1%磷酸溶液(20∶5∶75);流速:1.0 ml/min,检测波长:276 nm,柱温:35℃,进样量为10 μl.结果 甘草苷进样量在0.101 7～1.017 0 μg范围内时,与峰面积呈良好的线性关系(r＝0.999 95),平均回收率为99.31%,RSD=2.5%(n=6). 结论本方法简便、快速、准确,可作为该制剂的定量分析方法.     

HPLC法测定丁公藤注射液中东莨菪内酯含量

目的:建立高效液相色谱法测定丁公藤注射液含量的方法.方法:采用Sunfire柱(4.6 mm×150 mm,5 μm);流动相为甲醇-乙腈-冰醋酸(320:680:1.6);流量为 1.0 ml·min-1.检测波长为 298 nm.结果:进样量在20～60 μg·mL-1浓度时与峰面积呈良好线性关系,r=0.9983(n=5),平均回收率96.8%,RSD为0.94%.结论:该法简便、准确、结果可靠.     

高效液相色谱法测定氯法拉滨注射液中氯法拉滨的含量

目的:建立高效液相色谱法测定氯法拉滨注射液中主药氯法拉滨的含量.方法:采用Shim-pack VP-ODS(5 μm,4.6 mm ×150 mm)色谱柱,流动相为乙腈·乙酸铵溶液(取乙酸铵0.31 g,加水溶解并稀释至1000 mL,再加甲酸1.0 mE)(10:90),流速1.0 mL/min,进样量20μL,检测波长262 nm.结果:氯法拉滨在进样量0.4～242.5μg/mL范围内线性关系良好,回归方程为A=23156C+12378(r=0.9999,n=5),平均加样回收率为99.97%,RSD为0.40%.结论:本方法快速、简便、结果准确,可用于控制该制剂的质量.     

HPLC法测定十二太保丸中芍药苷的含量

目的:建立十二太保丸中芍药苷的含量测定.方法:色谱柱为Hypevsil ODS C18(200 mm×4.6 mm,5 λμm),流动相为乙腈-0.1%磷酸(15:85),流速1.0 ml·min-1,检测波长230 nm.结果:芍药苷在0.496～2.480 μg范围内峰面积与进样量呈良好的线性关系,平均加样回收率为99.7%,RSD为1.32%,n=6.结论:本方法简便、重现性好,可用于该制剂的质量控制.     

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.     

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.     

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.     

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.     

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.