HPLC法测定康媛颗粒中芍药苷的含量

目的探讨测定康媛颗粒中芍药苷含量的方法.方法色谱柱:采用高效液相色谱法(HPLC法),用十八烷基硅烷键合硅胶为填充剂4.6 mm×250 mm(5μ,Lichrospher,汉邦科技);流动相:乙腈-0.1%磷酸溶液(15:85);检测波长:232nm;柱温:40℃;流量:1.0 ml·min-1.结果芍药苷在0.198～1.188μg间成良好线性关系,回归方程为:Y=1050.2X-736.33;r=0.999 9,平均回收率为98.536%,RSD=3.0%.结论HPLC法可用于康媛颗粒的质量控制.     

芍药植株不同部位芍药苷含量分析

目的 检测芍药植株不同部位芍药苷含量的分布情况.方法 采用HPLC 法,色谱柱Shim pack vp-C18 5 μm,4.6 mm×150 mm柱,流动相为乙腈 0.1%磷酸溶液(14∶86),检测波长230 nm,流速1.0 ml·min-1.结果 芍药苷进样量在6.48～64.8 μg,在峰面积具有良好的线性关系,回归方程Y=12.51X-0.393(r=0.999),平均回收率98.60%,RSD为1.23%.芍药苷在不同部位中的含量分布为根茎＞根＞叶＞茎＞花.结论 该方法简便、快速、准确,重复性好.除了从芍药根部提取芍药苷,还可以从花、茎、叶,根茎提取芍药苷.     

HPLC法测定止痛胶囊中芍药苷的含量

目的　测定止痛胶囊中芍药苷的含量。方法　采用高效液相色谱法 ,色谱柱 :Nova pakC183 9mm× 15 0mm ;流动相 :0 1%磷酸 乙腈 (90∶10 ) ;流速 :1 0ml·min 1;检测波长 :2 30nm ;柱温 :2 0℃。结果　芍药甙在 30 6 2～ 30 6 2 0mg·ml 1范围内线性关系良好 (r=0 9996 )。日内、日间差RSD均不超过 3% (n =5 )。结论　该法可用于止痛胶囊中芍药苷含量的测定     

HPLC测定芍药丸中芍药苷的含量

目的 建立HPLC测定芍药丸中芍药苷含量的方法.方法 采用色谱柱为:Inertsil ODS-3C18(250 mm×4.6 mm,5μm);流动相:甲醇-1%磷酸溶液(35:65);柱温:40 ℃;流速:1.0 ml/min;检测波长为230 nm.结果 芍药苷含量在4.92～49.2 μg/ml,线性关系良好(r=0.999),平均回收率98.64%.结论 该法快速、简便、准确,可用于芍药丸的质量控制.     

HPLC法测定摩罗丹中芍药苷的含量

目的建立摩罗丹的质量控制方法。方法采用Agi-lent C18(150 mm×4.6 mm,5μm)色谱柱,以乙腈-0.05%磷酸二氢钾溶液(14∶86)为流动相,检测波长为230 nm;柱温:30℃;流速:1.0 m l·m in-1;测定摩罗丹中芍药苷的含量。结果芍药苷的线性范围为0.0872~0.872 mg·L-1(r=0.9996,n=5),平均回收率为98.6%(RSD=0.9%,n=6)。结论该方法简便、准确、专属性强,可有效控制摩罗丹的质量。     

HPLC法测定赤芍饮片中芍药内酯苷及芍药苷的含量

目的建立同时测定赤芍中芍药内酯苷和芍药苷含量的方法。方法采用高效液相色谱法。色谱柱:LichrosphereC18(4.6mm×250mm,5μm);流动相:甲醇-水(35∶65);流速:1.0mL.min-1;柱温:30℃;检测波长:230nm。结果芍药内酯苷和芍药苷分别在0.00788~0.15760μg(r=0.9999)和0.08356~1.67120μg(r=0.9999)范围内线性关系良好,平均加样回收率分别为93.85%和96.58%。结论该法快速、简便、准确、专属性强,可用于赤芍饮片的质量控制。     

反相高效液相色谱法测定胃炎片中芍药苷的含量

目的:建立胃炎片中芍药苷的含量测定方法。方法:采用反相高效液相色谱法测定胃炎片中芍药苷的含量。使用日本Sil C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1%磷酸水溶液(13:87)为流动相,流速为1 mL·min~(-1),检测波长230nm。结果:芍药苷进样量存0.14～1.40μg范围内线性关系良好,r=0.9994;平均回收率(n=9)为101.3%。结论:该方法简便、灵敏、准确,可作为胃炎片的质量控制方法。     

高效液相-质谱联用法不同色谱柱测定马钱苷和芍药苷的比较分析

目的:HPLC-MS法比较Phenomenex Kinetex C18(150 mm×4.6 mm,2.6μm)色谱柱、Wondasil C18(150 mm×4.6 mm,5μm)色谱柱对马钱苷和芍药苷分离效果。方法:以甲醇-0.02%甲酸(28∶72)为流动相;流速为0.7 mL.min-1;柱温30℃。先后采用2种不同色谱柱,对马钱苷和芍药苷标准溶液及含药血浆样品进行分析测定,比较其保留时间tR、理论塔板数N、拖尾因子Tf。结果:Phenomenex Ki-netex C18色谱柱和Wondasil C18色谱柱测定血浆样品马钱苷和芍药苷,保留时间分别为19.652、16.893 min(马钱苷)和18.467、19.459 min(芍药苷),理论塔板数分别为86 033、16 886(马钱苷)和81 342、17 523(芍药苷),拖尾因子分别为1.03、1.1(马钱苷)和1.02、1.13(芍药苷),2种色谱柱最低定量限分别为2.5 ng.mL-1和5 ng.mL-1。结论:Phenomenex Kinetex C18色谱柱,峰形尖锐,灵敏度较高,理论塔板数较大,但保留时间与Wondasil色谱柱相近。     

UPLC法测定郁舒片中5种药效成分含量

目的:建立UPLC法同时测定郁舒片中芍药内酯苷、芍药苷、芦丁、金丝桃苷、异槲皮苷的含量。方法:采用Waters Acquity UPLCTMBEH-C18(100 mm×2.1 mm,1.7μm)色谱柱,以0.1%磷酸水溶液(A)-乙腈(B)为流动相,梯度洗脱,流速0.4m L·min-1,检测波长203 nm,柱温30℃。结果:芍药内酯苷、芍药苷、芦丁、金丝桃苷、异槲皮苷5种成分在相应的范围内,呈良好的线性关系(r≥0.999 0);方法的平均加样回收率(n=6)分别为101.4%(RSD=0.82%)、101.9%(RSD=1.0%)、99.0%(RSD=2.6%)、98.9%(RSD=2.0%)、100.0%(RSD=2.4%)。3批样品的测定结果分别是芍药内酯苷3.53~3.80 mg·片-1,芍药苷9.33~10.01 mg·片-1,芦丁0.89~0.98 mg·片-1,金丝桃苷0.72~0.76 mg·片-1,异槲皮苷0.82~0.86 mg·片-1。结论:该方法分析时间短,操作简单,可以作为郁舒片的质量控制方法。     

超高效液相色谱法同时测定白芍中芍药苷和芍药内酯苷的含量

目的 采用超高效液相色谱法(UPLC)同时测定白芍中芍药苷和芍药内酯苷的含量.方法 采用Agilent Extend-C18(4.6 mm×50 mm,1.8μm)色谱柱,以流动相乙腈(A)-0.2％乙酸溶液(B)梯度洗脱;柱温30℃;流速0.5 mL·min-1;检测波长230 nm.结果 芍药苷和芍药内酯苷分别在0.011 6～1.45(r=0.999 9)、0.008～lmg·mL-1(r=0.999 9)呈良好的线性关系;平均回收率分别为98.6％、97.5％,RSD分别为1.4％、2.2％.结论 该法快速简便,灵敏度高,准确可靠,可用于白芍中有效成分含量的快速测定及白芍的质量控制.     

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.     

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.