高效液相色谱法测定红毛五加中绿原酸的含量

目的:采用LC／MS2方法鉴定出中药红毛五加中绿原酸成分,并用高效液相色谱法测定其含量。方法:采用Zorbax SB-C18色谱柱(150 mm×4．6mm,5μm);流动相为乙腈和水(含0．16％甲酸)二元梯度洗脱系统;流速为1．0mL·min-1,检测波长327 nm。质谱条件:Agilent多级离子阱质谱仪:电喷雾化学电离源(ESI);负离子检出模式。结果:绿原酸的线性范围为 10-100 mg·L-1(r=0.9997),加样回收率为99．2％-101．8％;红毛五加中绿原酸的含量为0．58-5．45mg．g-1。结论:本方法灵敏、快速、重现性好,有助于红毛五加质量控制方法的研究。     

RP-HPLC法测定川产藏药不同产地红毛五加茎皮中腺苷的含量

目的:建立藏药红毛五加药材中腺苷的含量测定方法并比较四川不同产地红毛五加的腺苷含量。方法:采用 KromasilC_(18)(250 mm×4.6 mm,5 μm)色谱柱,以乙腈-水溶液(5:95),流速1.0 mL·min~(-1);柱温25℃;检测波长为258 nm。结果:腺苷进样量在0.07～0.69 μg内呈良好的线性关系(r=0.9993),低、中、高3种加入量的平均加样回收率(n=3)分别为99.3%,99.1%,99.2%;RSD 均为0.9%。结论:本方法简便、准确,重复性好,可用于红毛五加的质量控制。     

RP-HPLC测定红毛五加中的异嗪皮啶

目的 建立测定红毛五加药材中异嗪皮啶的方法并比较不同药用部位及不同产地、不同采收期的红毛五加皮中异嗪皮啶的含量.方法 采用HPLC法,流动相为乙腈-甲醇-0.1%磷酸水溶液(20:10:70),流速为1 mL·min-1,检测波长为343 nm,柱温为25℃.结果 异嗪皮啶1.59×10-3～0.80 μg与峰面积具有良好的线性关系,回归方程为:Y=2.636×104X-1.051×103(r=0.9997,n=8),平均回收率为99.15%,RSD=0.95%(n=5).结论 所用方法简便、准确、重复性好,可控制红毛五加药材的质量.     

RP-HPLC测定3种五加皮中的绿原酸

目的采用HPLC测定五加科植物红毛五加、刺五加和萝藦科植物香加皮中的绿原酸,探讨其能否替代入药。方法采用Kromasil C18柱(250 mm×4.6 mm,5μm);柱温30℃;流动相为乙腈-2‰磷酸水溶液(10∶90);检测波长327 nm;流速1m.lmin-1。结果绿原酸的平均回收率为100.1%,RSD=0.9%。红毛五皮、刺五加皮、香加皮中绿原酸分别为:16.71、6.21、15.92 mg.g-1。结论所建方法简便、准确、重复性好,从化学成分绿原酸和香加皮毒性的角度考虑,建议不用3种药材替代入药,并应避免用香加皮代替五加皮类药材。     

HPLC测定细叶亚菊中的绿原酸

目的 采用HPLC测定细叶亚菊中的绿原酸含量.方法 采用Hypersil ODS-2柱(250 mm×4.6 mm,5 μm),流动相为甲醇-含0.04%磷酸的水溶液(19:81),流速1 mL·min~(-1),检测波长328 nm,柱温30℃.结果 绿原酸进样量的线性范围为0.0306～1.530 μg,与峰面积呈良好的线性关系(r=0.9999),平均回收率为99.7%,RSD=2.6%(n=5),细叶亚菊中绿原酸的含量为9.457 mg·g~(-1).结论 所建方法快速、简便、准确、重复性好,绿原酸可作为细叶亚菊的质量控制指标.     

UPLC法测定益智中的白杨素和圆柚酮

目的 采用超高效液相色谱法(UPLC)同时测定益智药材中的白杨素和圆柚酮.方法 色谱柱为Acquity UPLC BEH C18柱(100mm×2.1 mm,1.7 μm),流动相为乙腈-水溶液,流速0.2 mL· min-,采用梯度洗脱,检测波长251 nm.结果 白杨素0.139 ～347.5 μg·mL-1、圆柚酮0.197 ～ 492.5μg· mL-1与峰面积呈良好的线性关系(r2分别为0.9995、0.9994).平均加样回收率分别为98.97％(RSD=1.94％,n=9)、98.90％(RSD=1.45％,n=9).不同地区的益智和益智的不同部位中两种成分的含量均有明显差异.结论 所用方法准确、简单、重复性好,适用于益智中白杨素和圆柚酮的含量测定.     

HPLC测定通痹活络丸中的绿原酸

目的 采用RP-HPLC法测定通痹活络丸中绿原酸的含量.方法 采用Agilent Eclipse XDB C18柱(250 mm×4.6 mm,5 μm),流动相为乙腈-0.2％磷酸(9∶91),流速1.0 mL· min-1,检测波长327 nm,柱温35℃.结果 绿原酸0.0176～0.1756 μg与峰面积的线性关系良好(r=0.9999).平均加样回收率为101.5％,RSD =3.2％(n=9).结论 所用方法灵敏、准确、快速,重复性好,可用于通痹活络丸的质量控制.     

用高效凝胶色谱法测定红毛五加多糖组分的分子量

目的:采用高效凝胶色谱法测定红毛五加多糖分子量;方法:色谱柱为OHPak SB-805HQ(8 mm×300mm),以高纯水为流动相,流速0.8 ml·min-1,柱温35℃,示差折光器检测.结果:AGP1分子量为91 000;AGP2分子量为85 000;AGP3分子量为45 000.结论:红毛五加多糖分子量在91 000～45 000之间,由AGP1、AGP2、AGP3三种组分组成.     

HPLC测定紫蒲痛风合剂中的绿原酸

目的 采用HPLC法测定紫蒲痛风合剂中绿原酸的含量.方法 采用Waters Symmetry Shield RP18色谱柱(250 mm×4.6 m1m,5μm),流动相为乙腈-0.4％磷酸溶液(10∶90),流速1.0 mL· min-1,检测波长327 nm.结果 67.2 ～ 806.4 ng绿原酸与峰面积呈良好的线性关系(r=0.9999),平均加样回收率为115.54％,RSD =0.92％ (n =6).结论 所用方法准确、简便、可靠,可用于该制剂的质量控制.     

HPLC法测定复方鱼腥草合剂中绿原酸、黄芩苷的含量

目的:建立同时测定复方鱼腥草合剂中绿原酸、黄芩苷的高效液相色谱法.方法:采用Sinochrom ODS-BP(250 mm×4.6 mm,5 μm)色谱柱;流动相为甲醇:0.2%磷酸溶液,进行梯度洗脱;柱温:30℃流速为0.9 ml·min-1,检测波长为315 nm.结果:绿原酸在0.1～1.0 μg·ml-1范围内线性关系良好(r=0.999 5),平均回收率为100.26%,RSD=0.53%(n=9);黄芩苷在1.8～18.0 μg·ml-1范围内线性关系良好(r=0.996 6),平均回收率为100.04%,RSD=0.87%(n=9).结论:本方法简便易行,能够准确、快速测定复方鱼腥草合剂中的绿原酸和黄芩苷的含量.     

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.     

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.