HPLC-ELSD法测定芪心合剂中黄芪甲苷的含量

目的建立高效液相色谱-蒸发光散射检测(HPLC-ELSD)法测定芪心合剂中黄芪甲苷含量测定的方法。方法色谱柱为Waters-SunFire C18(250 mm×4.6 mm,5μm);柱温为35℃;流动相为乙腈-水(40∶60);流速为1.0 ml.min-1;ELSD检测器参数:雾化器温度36℃,漂移管温度为60℃,空气压力为30.0 psi。结果黄芪甲苷进样量在0.98～9.78μg范围内与峰面积线性关系良好(r=0.999 7,n=5),平均加样回收率为99.78%,RSD为0.5%(n=6)。结论该方法简便、结果可靠,可作为芪心合剂中黄芪甲苷含量的测定方法。     

消白颗粒的质量标准提升研究

目的 建立并提升消白颗粒制剂的质量标准。方法 采用TLC对消白颗粒中的黄芪、地黄、首乌、补骨脂进行定性鉴别;采用HPLC-ELSD测定制剂中黄芪甲苷的含量。色谱条件：Lichrospher-C₁₈柱(4.6 mm×250 mm,5 mm),以乙腈-水(32∶68)为流动相,流速 1.0 mL·min^-1,柱温 25 ℃,蒸发光散射检测器检测。结果 消白颗粒中黄芪、地黄、首乌、补骨脂的TLC斑点清晰,分离度良好,阴性无干扰。黄芪甲苷在0.311 5~2.803 9 μg(r=0.999 9)内呈良好的线性关系,平均回收率为99.4%(RSD=2.67%)。结论 该方法简便、准确、重复性好,可作为消白颗粒的质量标准。     

HPLC-蒸发光散射检测法测定复方芪葜颗粒中黄芪甲苷的含量

目的:建立高效液相色谱-蒸发光散射检测法测定复方芪葜颗料中黄芪甲苷的含量。方法:色谱柱:AgilentHypersilODS柱(4.0×250mm,5μm),流动相:甲醇-水(70∶30),流速:1mL/min,检测器:AlltechELSD-2000,漂移管温度:85℃,气体流速:2.0L/min。结果:黄芪甲苷在1.98～9.90μg范围内呈线性,(r=0.9999n=5)回收率97.3%(RSD=1.90n=5)。结论:方法简便,结果可靠,可作为复方芪葜颗粒中黄芪甲苷的含量的定量方法。     

HPLC-ELSD法测定芪蛭降糖颗粒中黄芪甲苷的含量

目的:建立高效液相色谱-蒸发光散射检测法(HPLC-ELSD)测定芪蛭降糖颗粒中黄芪甲苷含量的方法。方法:色谱柱为Hypersil ODS2柱(250 mm×4.6 mm,5μm),流动相为乙腈-水(32∶68),流速为1.0 mL·min-1,进样量为10μL,柱温为25℃。ELSD条件为漂移管温度110℃;气体流量为3.12 SLPM。结果:以浓度的常用对数(C)对其相应峰面积常用对数(A)进行回归分析,得回归方程为A=1.699 C+6.181,r=0.999 6(n=5);样品浓度在0.259～1.295 mg·mL-1范围内与峰面积积分值线性关系良好;最低检测限为5.18μg·mL-1;平均加样回收率为97.75%,RSD=2.17%。结论:采用PLC-ELSD法测定芪蛭降糖颗粒中黄芪甲苷含量,方法简便快捷,测定结果可靠,可用于芪蛭降糖颗粒的质量控制。     

高效液相色谱-蒸发光散射检测器法测定仙芪眩宁颗粒中黄芪甲苷含量

目的建立仙芪眩宁颗粒中黄芪甲苷的含量测定方法。方法采用高效液相色谱-蒸发光散射检测器法,色谱柱为Phenomenex GeminiC18柱(250 mm×4.6 mm,5μm),流动相为甲醇-水(80∶20),流速1.0 mL/min,柱温30℃,进样量10μL;蒸发光散射检测器漂移管温度为45℃,载气(空气)流速3.0 L/min。结果黄芪甲苷进样量在25.52～127.6μg范围内的对数值与峰面积的对数值线性关系良好,r=0.999 3,平均回收率为96.89%,RSD为1.44%(n=6)。结论该方法无干扰,准确、重现性良好,可作为产品的质量控制方法。     

HPLC-ELSD法测定芪参咀嚼片中黄芪甲苷的含量

目的建立采用高效液相色谱—蒸发光散射检测器法(HPLC-ELSD)测定芪参咀嚼片中黄芪甲苷含量的方法。方法采用Kromasil C18(250.0mm×4.6mm,5μm)的色谱柱;以乙腈—水(38:62)为流动相;流速:1ml/min;ELSD检测条件:检测器漂移管温度为80℃,氮气压力为0.24MPa,柱温为30℃。结果黄芪甲苷在2.55～15.30μg范围内与峰面积分别取自然对数后呈良好的线性关系(r=0.9996,n=6),平均回收率是99.82%(RSD=0.2%)。结论 HPLC-ELSD法测定芪参咀嚼片中黄芪甲苷含量简便、准确、可靠,可作为该制剂的含量测定方法。     

HPLC测定清流颗粒中的黄芪甲苷

目的 采用HPLC法测定清流颗粒中的黄芪甲苷.方法 采用Agilent C18色谱柱(150 mm×4.6mm,5μm),流动相为乙腈-水(32:68),流速0.8 mL·min-,柱温35℃,ELSD漂移管温度101℃,载气流速2.8 L·min-1.结果 黄芪甲苷1.032 ～5.160 μg与峰面积的线性关系良好,回收率为93.49％,RSD=1.95％ (n =6).结论 所用方法具有良好的精密度和重复性,可用于测定清流颗粒中的黄芪甲苷.     

HPLC-ELSD法测定芪蛭降糖片中黄芪甲苷的含量

目的:建立用高效液相色谱-蒸发光散射检测器测定芪蛭降糖片中黄芪甲苷含量的方法.方法:色谱柱为Lichrospher 5 C18柱(4.6 mm×250 mim,5 μm),流动相为乙腈-水-四氢呋喃(33:67:4),流速为1.0 mL/min,ELSD参数中漂移管温度为110℃,N2流速为2.84 mL/min.结果:黄芪甲苷线性范围是2.016～12.096 μg,r=0.999 7;平均加样回收率为99.3%,RSD为2.3%.结论:该方法简便、可靠,可作为芪蛭降糖片的质量控制方法.     

HPLC-蒸发光散射检测法测定贞芪扶正颗粒中黄芪甲苷的含量

目的:建立高效液相色谱-蒸发光散射检测法测定贞芪扶正颗粒中黄芪甲苷含量的方法。方法:色谱柱为Hypersil ODS2 C18(200mm×4.6mm,5μm),流动相为乙腈-水(35∶65),流速为1mL·min-1,载气为氮气(N2),气体压力为1.5MPa,雾化温度为35℃,气化温度为50℃。结果:黄芪甲苷进样量在2.38~51.00μg范围内的对数值与峰面积对数值呈良好线性关系;平均回收率为100.71%,RSD=1.94%(n=6)。结论:本方法迅速、准确、重现性好,可用于贞芪扶正颗粒的质量控制。     

芪葵颗粒定性定量方法研究

目的:建立芪葵颗粒的定性定量方法。方法:用薄层色谱法对该颗粒中的黄芪、黄蜀葵花、制何首乌进行定性鉴别。采用HPLC-ELSD法测定制剂中黄芪甲苷,使用Hedera ODS-2(4.6 mm×250 mm,5μm)色谱柱,以乙腈-水(32∶68)为流动相,流速1.0 mL.min-1,柱温30℃,Alltech 2000ES蒸发光散射检测器(漂移管温度102℃,载气流量2.8 L.min-1);采用HPLC法测定制剂中金丝桃苷、2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷(简称二苯乙烯苷)的含量,使用HederaODS-2(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.1%磷酸水溶液为流动相进行梯度洗脱,流速1.0 mL.min-1,检测波长320 nm,柱温30℃。结果:在薄层色谱中均能检出黄芪、黄蜀葵花、制何首乌。黄芪甲苷、金丝桃苷、二苯乙烯苷线性范围分别为1.59～21.3μg(r=0.9997),0.048～0.567μg(r=0.9999),0.054～0.625μg(r=1.000);平均回收率(n=6)分别为95.0%(RSD=2.2%),104.0%(RSD=1.3%),101.5%(RSD=1.4%)。结论:所建方法简便、准确,重复性好,可作为复方芪葵颗粒的定性定量方法。     

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.