HPLC法测定杞菊地黄软胶囊中芍药苷的含量

目的建立杞菊地黄软胶囊中芍药苷的含量测定方法。方法采用高效液相色谱法测定该药中芍药苷的含量,色谱条件:汉邦科技有限公司,Kromasil C18(5μm,4.6 mm×250 mm)为色谱柱,甲醇∶0.1%三氟乙酸水溶液(24∶76)为流动相;流速1.0 ml.min-1;检测波长:230 nm。结果芍药苷浓度范围在22~704 mg.L-1之间峰面积与浓度线性关系良好,r=0.999 8平均回收率100.34%,RSD=0.85%。结论该方法准确、可靠、专属性强,可用于杞菊地黄软胶囊的质量控制。     

HPLC测定杞菊地黄胶囊中的丹皮酚

目的 建立测定杞菊地黄胶囊中丹皮酚的方法.方法 采用HPLC法,Shim-pack VP-C18色谱柱(4.6 mm×150 mm,5 μm),流动相为甲醇-水(60:40),流速1.0 ml·min-1,检测波长274 nm,柱温35℃,进样量10 μl.结果 线性范围0.03～2.30 μg(r＝0.9998),平均回收率100.38%,RSD＝1.89%(n＝9).结论 所建方法分离度好、快速、简便,适用于杞菊地黄胶囊中丹皮酚的含量测定,可作为产品的质量控制方法.     

HPLC法测定杞菊地黄丸中莫诺苷、马钱苷和丹皮酚的含量

目的:建立一种快速、准确和实用的HPLC方法,用于同时测定杞菊地黄丸中莫诺苷、马钱苷和丹皮酚的含量。方法:采用Phenomenex Gemini C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.3%磷酸水溶液为流动相梯度洗脱,流速1.0 m L·min-1,柱温40℃,检测波长为240 nm(莫诺苷、马钱苷)和274 nm(丹皮酚)。结果:莫诺苷、马钱苷、丹皮酚质量浓度分别在2.242~44.84μg·m L-1(r=0.999 9)、2.130~42.60μg·m L-1(r=1.000)、5.068~101.4μg·m L-1(r=1.000)范围内,与峰面积线性关系良好;平均回收率分别为96.2%(RSD=0.44%)、96.0%(RSD=0.21%)、103.0%(RSD=0.65%)。结论:本方法可作为杞菊地黄丸中莫诺苷、马钱苷和丹皮酚含量同时测定的方法,适用于杞菊地黄丸的质量控制。     

毛细管气相色谱法测定杞菊地黄丸(浓缩丸)中丹皮酚的含量

目的建立毛细管气相色谱法测定杞菊地黄丸（浓缩丸）中丹皮酚含量的方法。方法色谱柱为HP-5石英毛细管柱（30m×0．32mm×0．25μm）;氢火焰离子化检测器;色谱条件：柱温130℃、进样口温度250℃、检测器温度250℃;分流进样：分流比：5：1。按外标法测定丹皮酚的含量。结果丹皮酚在105．9～1059．0mg·L^-1浓度范围内与峰面积线性关系良好（r=0．9998）,平均加样回收率为97．7％（RSD=0．7％,n=6）。结论本法准确、可靠、快速、简便,可用于测定杞菊地黄丸（浓缩丸）中丹皮酚的含量。     

杞菊地黄口服液的质量标准提高研究

目的:为完善和提高杞菊地黄口服液的质量标准提供参考。方法:根据2015年版《中国药典》(四部)0502法对杞菊地黄口服液中枸杞子、菊花、牡丹皮进行薄层色谱(TLC)鉴别,分别以枸杞子、菊花和丹皮酚为对照,展开系统分别为三氯甲烷-乙酸乙酯-甲酸(6∶1∶0.5,V/V/V)、三氯甲烷-异丙醇-甲酸(10∶1∶0.5,V/V/V)和环己烷-乙酸乙酯(3∶1,V/V);采用高效液相色谱法(HPLC)同时测定杞菊地黄口服液中莫诺苷、马钱苷及丹皮酚的含量[色谱柱为InertSustain C_(18),流动相为乙腈-0.03%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长分别为240 nm(莫诺苷和马钱苷)和274 nm(丹皮酚),柱温为40℃,进样量为10μL]。结果:在枸杞子、菊花、牡丹皮TLC供试品图谱中,与对照药材/对照品图谱相应的位置上显相同颜色的斑点,且阴性对照无干扰。莫诺苷、马钱苷及丹皮酚检测质量浓度的线性范围分别为2.12～106.17、1.91～95.63、4.78～239.16μg/mL(R~2=0.999 9、0.999 9、0.999 8);定量限分别为2.12、1.91、2.39μg/mL;检测限分别为0.53、0.48、0.59μg/mL;精密度、重复性、稳定性试验的RSD均小于2%(n=6);平均回收率分别为98.27%、97.06%、97.65%,RSD分别为0.80%、1.18%、1.36%(n=6);耐用性试验的RSD均小于2%(n=3)。结论:本研究建立的方法操作简便、专属性强、耐用性好,可为完善杞菊地黄口服液的质量标准提供一定参考。     

HPLC法测定明目地黄胶囊中丹皮酚的含量

目的建立明目地黄胶囊中丹皮酚的含量测定方法。方法采用高效液相色谱法,以Hypersil BDSC18（5μm,4．6mm×250mm）为色谱柱;以甲醇：水（60：40）为流动相;检测波长：274nm;流速：0．8ml·min^-1。结果丹皮酚在0．512—10．24mg·L^-1范围内线性关系良好,r=0．9997,平均回收率为100．6％,RSD为1．3％。结论该方法快速、准确、重复性好,可用于明目地黄胶囊中丹皮酚的含量测定。     

HPLC法测定利心丸中丹皮酚的含量

目的: 建立HPLC法测定利心丸中丹皮酚的含量测定方法.方法: 色谱柱为AllfimaCl8(250mm×4.6mm;5μm),以甲醇-水(60:40)为流动相,流速为1.Oml·min-1检测波长274nm,结果: 丹皮酚的线性范围是5.2～41.1μg·ml-1,r=0.9998,平均加样回收率为98.7%,RSD为0.9%.结论: 该方法结果准确、重复性好,可用于该制剂的质量控制.     

知柏地黄泡腾颗粒的质量标准研究

目的:建立知柏地黄泡腾颗粒的质量标准。方法:采用TLC方法对知柏地黄泡腾颗粒中牡丹皮、山茱萸、黄柏进行定性鉴别;采用HPLC法测定了马钱苷和丹皮酚的含量,色谱柱为Hypersil C18柱(250mm×4.6 mm,5μm),马钱苷的流动相为乙腈-水(14∶86),流速为1.0 mL.min-1,检测波长为240 nm。丹皮酚的流动相为甲醇-0.1%磷酸溶液(47∶53),流速为1.0 mL.min-1,检测波长为274 nm。结果:TLC法可检出牡丹皮、山茱萸、黄柏,斑点清晰,阴性对照无干扰,专属性强。马钱苷的平均加样回收率为99.14%,RSD为0.87%。线性范围为0.181 2~1.359 0μg(r=0.999 9)。丹皮酚的平均加样回收率为101.21%,RSD为2.00%。线性范围为0.099~0.495μg(r=0.999 6)。结论:本方法准确可靠,可作为知柏地黄泡腾颗粒的质量控制方法。     

RP-HPLC法同时测定复方益肾软胶囊中盐酸巴马汀、盐酸小檗碱和丹皮酚的含量

目的:建立同时测定复方益肾软胶囊中盐酸巴马汀、盐酸小檗碱和丹皮酚含量的方法。方法:采用反相高效液相色谱法。色谱柱为Diamonsil-C1(8200mm×4.6mm,5μm),流速为1mL.min-1,流动相为乙腈-0.03mol.L-1磷酸二氢钾缓冲溶液(pH3.10,梯度洗脱),检测波长为265nm,进样量为20μL。结果:盐酸巴马汀、盐酸小檗碱和丹皮酚进样量的线性范围分别为0.01661～0.41520μg(r=0.9999)、0.02701～0.67520μg(r=0.9999)、0.15700～1.25570μg(r=0.9999);平均加样回收率分别为99.81%(RSD=0.82%,n=6)、99.53%(RSD=0.74%,n=6)、98.32%(RSD=0.87%,n=6)。结论:本方法操作简便、准确、重复性好,可作为复方益肾软胶囊的质控方法。     

HPLC测定丹皮酚软膏（丹皮酚霜）中丹皮酚的含量

目的:采用 HPLC 法测定丹皮酚软膏(霜)中丹皮酚的含量。方法:色谱柱为 Hypersil C_(18)柱(150 mm×4.6 mm,5 μm);流动相:甲醇-水(50:50);流速1.0 mL·min~(-1);检测波长:274 nm。结果:丹皮酚进样量在0.05～0.54 μg范围内呈良好线性关系(r=0.9998),平均回收率(n=6)为98.7%,RSD 为2.0%。结论:本法准确,重现性好。     

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.