HPLC法同时测定杏花中阿魏酸、芦丁和异槲皮苷

目的建立HPLC法同时测定杏花中阿魏酸、芦丁和异槲皮苷。方法色谱柱为YMC-Pack ODS-A C_(18)柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.1%磷酸溶液(15∶85);体积流量1.0 mL/min;检测波长为343 nm;柱温为30℃。结果阿魏酸、芦丁和异槲皮苷分别在0.029 08~0.290 8μg(r=0.999 9)、0.548 4~5.484 2μg(r=0.999 9)、0.033 07~0.330 7μg(r=0.999 9)范围内线性关系良好;平均回收率分别为98.31%、98.93%、100.25%,RSD分别为1.0%、0.9%、1.1%。10批杏花样品中阿魏酸、芦丁、异槲皮苷含量测定结果分别为0.105~0.554、3.080~6.933、0.258~0.974 mg/g。结论该方法多种成分同时测定,操作简便、准确,重复性好,可用于杏花药材的质量控制。     

HPLC法同时测定金钮扣中芦丁和异槲皮苷的含量

目的建立以高效液相色谱法同时测定金钮扣中芦丁和异槲皮苷含量的方法。方法色谱柱为Agela Promosil C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-质量分数为0.2%的磷酸溶液(体积比为15:85),流速为1.0 mL·min^(-1),检测波长为360 nm,柱温为35℃。结果芦丁和异槲皮苷的质量浓度分别在0.032～1.920 mg·L(-1),检测波长为360 nm,柱温为35℃。结果芦丁和异槲皮苷的质量浓度分别在0.032～1.920 mg·L^(-1)(r=0.999 5)和0.800～48.000 mg·L(-1)(r=0.999 5)和0.800～48.000 mg·L^(-1)(r=0.999 5)内与峰面积呈良好的线性关系;平均回收率分别为99.2%和99.7%,RSD分别为1.0%和1.5%。结论本方法可作为金钮扣的质量控制方法之一。     

HPLC法同时测定川楝子中芦丁、异槲皮苷和槲皮素的含量

目的:采用高效液相色谱法同时测定川楝子药材中芦丁、异槲皮苷和槲皮素的含量。方法:采用Agilent Zorbax SB-C18(4.6 mm×150 mm,5μm)色谱柱,以甲醇-乙腈(1∶10)为流动相A,0.4%磷酸溶液为流动相B,梯度洗脱;流速1.0 mL.min-1;检测波长360 nm;柱温25℃。结果:芦丁、异槲皮苷和槲皮素浓度在5.0～500.0μg.mL-1(r=0.9995)、0.5～50.0μg.mL-1(r=0.9999)、1.0～100.0μg.mL-1(r=0.9996)范围内与峰面积呈良好的线性关系;平均加样回收率(n=9)分别为96.5%、97.4%、96.3%。所测22份川楝子药材中,芦丁、异槲皮苷和槲皮素的含量范围分别为19.82～120.21、1.43～38.12、4.30～20.48μg.g-1。结论:不同购买地川楝子药材中3个黄酮类成分含量差异较大;该方法适用于川楝子中3个黄酮的含量测定。     

HPLC法测定舒肝解郁胶囊中芦丁、金丝桃苷、异槲皮苷的含量

目的:建立舒肝解郁胶囊中芦丁、金丝桃苷、异槲皮苷三种成分的含量测定方法。方法:采用三元梯度HPLC法同时测定芦丁、金丝桃苷、异槲皮苷的含量。色谱柱:AQ Welch C_(18)(4.6×250 mm,5μm);流动相:甲醇(A)-乙腈(B)-0.1%磷酸(C);流速:0.6 ml/min;检测波长:360 nm。结果:芦丁、金丝桃苷、异槲皮苷的线性范围依次为:0.0437μg~3.6417μg(r=0.9999),0.0380μg~3.7973μg(r=0.9999),0.0157μg~3.28μg(r=0.9991):平均回收率(n=6)依次为:102.1%(RSD=0.69%),99.9%(RSD=1.23%),102.6%(RSD=1.98%)。结论:本方法简便、准确、分离度高,重现性好。     

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。     

HPLC测定新疆药桑叶中绿原酸、芦丁、异槲皮苷和槲皮素

目的建立新疆药桑叶中绿原酸、芦丁、异槲皮苷和槲皮素的高效液相色谱测定方法。方法采用BDS C18色谱柱（4.6 mm×250 mm,5μm）,柱温：25℃,流动相：乙腈（A）-0.01 mol.L-1醋酸铵溶液（100 mL中含0.2 mL三乙胺,用冰醋酸调pH至4.8）（B）,梯度洗脱[0 min,A-B（8∶92）;30 min,A-B（30∶70）],流速：1.0 mL.min-1,检测波长350 nm。结果绿原酸在1.052 0μg～5.067 9μg（r=0.999 3）、芦丁在1.029 4μg～5.031 7μg（r=0.999 8）、异槲皮苷在1.076 8～5.065 5μg（r=0.999 0）、槲皮素在1.075 0μg～5.055 0μg（r=0.999 1）内线性关系良好。绿原酸、芦丁、异槲皮苷和槲皮素的平均回收率分别为102.2%（RSD=1.3%）、104.6%（RSD=0.9%）、104.0%（RSD=1.9%）、104.7%（RSD=1.2%）。检出限（S/N=3）分别为0.160,0.081,0.033,0.640μg.mL-1。结论此法操作简便、快速、灵敏、准确,样品处理简便易行,适于同时测定新疆药桑叶中绿原酸、芦丁、异槲皮苷和槲皮素。     

高效液相色谱法同时测定田基黄注射液中槲皮苷、异槲皮苷的含量

目的:建立以高效液相色谱法同时测定田基黄注射液中槲皮苷、异槲皮苷含量的方法。方法:色谱柱为MerckLichrospher RP18,流动相为乙腈-(pH=3.0)磷酸盐缓冲液(18∶82),流速为1ml/min,柱温为25℃,检测波长为350nm。结果:槲皮苷、异槲皮苷进样量分别在0.278μg～4.440μg(r=0.9991)、0.315μg～2.520μg(r=0.9991)范围内与峰面积积分值线性关系良好;平均加样回收率分别为98.60%(RSD=2.23%)、97.79%(RSD=1.74%)。结论:本方法准确可靠、应用性强,可用于本品的质量控制。     

HPLC法同时测定杜仲叶中8种成分的含量

目的:建立同时测定杜仲叶中桃叶珊瑚苷、京尼平苷酸、儿茶素、绿原酸、车叶草苷、芦丁、异槲皮苷和紫云英苷等8种成分的含量测定方法。方法:采用高效液相色谱法。色谱柱为Agilent ZORBAX SB-C18,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为203 nm(桃叶珊瑚苷、儿茶素)、239 nm(京尼平苷酸、车叶草苷)、220 nm(绿原酸)、354 nm(芦丁、异槲皮苷)、266 nm(紫云英苷),进样量为5μL。结果:桃叶珊瑚苷、京尼平苷酸、儿茶素、绿原酸、车叶草苷、芦丁、异槲皮苷和紫云英苷的线性范围分别为0.812～6.090μg(r=0.999 3)、0.438～3.285μg(r=0.999 2)、0.045～0.336μg(r=0.999 2)、0.882～6.615μg(r=0.999 3)、0.097～0.726μg(r=0.999 1)、0.064～0.483μg(r=0.999 3)、0.048～0.360μg(r=0.999 1)、0.014～0.108μg(r=0.999 7);精密度、重复性和稳定性试验的RSD均小于3.5%(n=6);平均加样回收率分别为101.60%、103.06%、99.77%、96.93%、98.17%、96.75%、98.97%、99.60%,RSD分别为1.42%、2.65%、2.78%、2.05%、2.26%、0.93%、2.79%、3.08%(n=6)。不同采集时间、不同种植品种的12批杜仲叶样品中桃叶珊瑚苷、京尼平苷酸、儿茶素、绿原酸、车叶草苷、芦丁、异槲皮苷和紫云英苷的含量范围分别为10.903～17.245、5.578～7.892、0.198～0.440、13.890～19.782、1.008～1.547、1.102～2.396、0.267～0.701、0.150～0.412 mg/g,含量波动较大;杜仲皮样品中桃叶珊瑚苷、京尼平苷酸、儿茶素、绿原酸、芦丁、松脂醇二葡萄糖苷的含量分别为0.299、0.123、0.580、0.112、0.026、1.961 mg/g。结论:本方法操作简便、重复性好、准确度高,可用于评价杜仲叶的质量;不同采集时间、不同种植品种的杜仲的不同药用部位(皮、叶)中的成分组成及含量存在明显的差异。     

HPLC测定双山颗粒剂中绿原酸、芦丁和槲皮苷的含量

目的:建立双山颗粒中绿原酸、芦丁和槲皮苷3种成分的HPLC含量测定方法。方法:色谱柱采用Diamonsil C18(2)柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.2%磷酸溶液,梯度洗脱;检测波长为355 nm;柱温为25℃;流速为1.0 mL.min-1。结果:绿原酸、芦丁和槲皮苷的线性范围分别为0.106～0.636μg(r=0.999 7),0.035 3～0.211μg(r=0.999 4)和0.030 4～0.243μg(r=0.999 5);3成分的平均回收率在99.0%～100.1%。结论:该法简便、准确、重复性好,可用于双山颗粒剂的质量控制。     

RP-HPLC法测定鱼腥草生药中4种黄酮类化合物的含量

目的:建立 HPLC 测定鱼腥草生药中芦丁、金丝桃苷、槲皮苷和槲皮素含量的定量分析方法。方法:HPLC 外标法。采用色潜柱:Kromasil—C_(18)柱(250 mm×4.6 mm,10 μm);流动相1:水-乙睛-磷酸(400:100:0.2),30 min 时手动切换为流动相2:乙腈-甲醇-水-磷酸(375:75:50:0.1);检测波长350 nm;流速1.0 mL·min~(-1);柱温:室温。结果:在上述色谱条件下,芦丁、金丝桃苷、槲皮苷和槲皮素获良好分离,进样量分别在0.055～0.550μg(r=0.9979)、0.248～2.480μg(r=0.9977)、0.52～5.200μg(r=0.9998)和0.062～0.623μg(r=0.9961)范围内与其峰面积线性关系良好,加样回收率分别为103.5%,104.0%,102.6%,103.7%,重复性试验 RSD 分别为3.9%,0.8%,1.0%,1.6%。结论:该方法分离度好,简便快速,为鱼腥草生药及其制剂的质量控制提供可借鉴的分析办法。     

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.     

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.     

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.