田基黄药材的质量研究

目的建立田基黄药材的薄层色谱鉴别法以及其中槲皮苷和异槲皮苷HPLC含量测定方法,考察不同产地、不同采收期的药材质量。方法以槲皮苷、异槲皮苷为对照品,采用聚酰胺薄膜层析法对田基黄药材进行定性;采用高效液相色谱法,以Merck lichroCART RP-18e(250 mm×4.0 mm,5μm)为色谱柱,乙腈-磷酸盐缓冲液pH=3(18∶82)为流动相,检测波长为350 nm进行定量。结果加样回收率槲皮苷97.79%、RSD为1.53%,异槲皮苷97.23%、RSD为2.06%。结论本方法简便、快速,专属性强,分离度好,重现性好。     

莲须的UPLC指纹图谱及异槲皮苷含量分析

目的 建立莲须的超高效液相色谱法(UPLC)指纹图谱，并建立其异槲皮苷的含量测定方法。方法 色谱柱为Waters Acquity UPLCHSS T3,1.8μm, 2.1×100 mm;以乙腈(A)-0.2%乙酸(B)为流动相进行梯度洗脱；流速0.2 mL·min^-1;柱温：30℃;进样量3μL;检测波长300 nm。建立莲须药材的指纹图谱和异槲皮苷含量分析方法，并对19批不同产地莲须药材进行测定。结果 指纹图谱及含量测定方法的各项方法学验证均良好，19批莲须与对照指纹图谱的相似度在0.883～0.995,标定了7个共有峰。主要成分异槲皮苷线性关系良好(R²>0.999),加样回收率在91.58%～99.70%,RSD为3.54%,19批莲须异槲皮苷含量在0.011%～0.033%。结论 所建立的莲须UPLC指纹图谱及异槲皮苷含量分析方法专属性强、分离度好、灵敏度高，可为莲须药材的质量控制与评价提供参考。     

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。     

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。     

高效液相色谱法同时测定不同产地枳壳药材中柚皮苷、橙皮苷、新橙皮苷、异柚皮苷的含量

目的建立同时测定枳壳药材中柚皮苷、橙皮苷、新橙皮苷、异柚皮苷含量的方法。方法采用高效液相色谱法,色谱柱VenusilXBP C18柱（250 mm×4.6 mm,5μm）,流动相为乙腈-0.1%甲酸（梯度洗脱）,检测波长为283 nm,流速为1 mL/min;柱温为30℃。结果柚皮苷进样量在0.5～5μg范围与峰面积线性关系良好,r=0.999 8;异柚皮苷在0.08～2.01μg范围线性良好,r=0.999 8;橙皮苷在0.06～1.2μg范围线性关系良好,r=0.999 9;新橙皮苷在0.09～4.82μg范围线性关系良好,r=0.999 7。异柚皮苷、柚皮苷、橙皮苷和新橙皮苷平均加样回收率分别为101.17%,98.25%,95.42%和100.95%。结论该方法简便、准确、可靠,适用于枳壳药材质量控制。     

一测多评法同时测定芒果止咳片中6种药效成分的含量

目的:建立同时测定芒果止咳片中没食子酸、原儿茶酸、芒果苷、高芒果苷、金丝桃苷和异槲皮苷含量的方法。方法:采用高效液相色谱法。色谱柱为Phenomenex Gemini C18,流动相为0.1%磷酸水溶液-乙腈(梯度洗脱),流速为1.0 mL/min,检测波长为258 nm,柱温为30℃,进样量为5μL。以没食子酸为内参物,计算原儿茶酸、芒果苷、高芒果苷、金丝桃苷和异槲皮苷的相对校正因子,并将一测多评法与外标法测定结果进行比较。结果:没食子酸、原儿茶酸、芒果苷、高芒果苷、金丝桃苷和异槲皮苷检测质量浓度的线性范围分别为45.75～1 830μg/m L(r=0.999 9)、2.525～101.0μg/mL(r=0.999 9)、65.33～2 613μg/m L(r=0.999 6)、9.058～362.3μg/mL(r=0.999 9)、3.885～155.4μg/mL(r=0.999 9)、1.870～74.8μg/mL(r=0.999 9);定量限分别为0.571、0.643、1.053、0.854、0.830、1.500μg/mL,检测限分别为0.171、0.193、0.316、...     

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法同时测定辣木叶颗粒中异槲皮苷、紫云英苷和丹酚酸B的含量

目的:建立同时测定辣木叶颗粒中异槲皮苷、紫云英苷和丹酚酸B含量的方法。方法:采用高效液相色谱(HPLC)法。色谱柱为Cosmosil-C_(18),流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.3 mL/min,柱温为40℃,检测波长为260 nm,进样量为10μL。结果:异槲皮苷、紫云英苷和丹酚酸B检测质量浓度线性范围分别为0.017～0.341、0.010～0.194、0.010～0.195 mg/mL(r均>0.999 0);检测限分别为0.085、0.143、0.117μg/m L;定量限分别为0.283、0.476、0.392μg/mL;精密度、稳定性(24 h)、重复性试验的RSD均≤2.0%(n=6);平均加样回收率分别为101.22%、98.76%、98.72%,RSD分别为0.66%、0.30%、0.30%(n=6)。结论:建立的方法简便、准确、重复性好,可用于同时测定辣木叶颗粒中异槲皮苷、紫云英苷和丹酚酸B的含量。     

高效液相色谱法测定异叶爬山虎中异槲皮苷的含量

目的 建立高效液相色谱法(HPLC)测定异叶爬山虎中异槲皮苷含量的方法,并测定广西不同地区的异叶爬山虎中异槲皮苷的含量.方法 采用Inersil-C18色谱柱(4.6 mm×25 mm,5μm),流动相为甲醇-0.05%磷酸溶液(46:54),流速1 mL·min-1,检测波长258 nm,柱温25℃,进样量10μL,分析时间32 min.结果 异槲皮苷的进样量在20~200μg范围内,与峰面积呈良好的线性关系,相关系数r=0.9999(n=6);异槲皮苷的平均回收率为98.53%(n=6),RSD为0.79%.结论 该法操作简便,重复性好,可用于测定异叶爬山虎中异槲皮苷含量.     

HPLC法测定铁扫帚药材中槲皮苷含量的方法研究

目的建立铁扫帚药材中槲皮苷含量的高效液相色谱测定法。方法采用C18色谱柱(4.6 mm×150mm,5μm),以甲醇-0.01 mol.L-1磷酸二氢钾-冰醋酸(35∶63.5∶1.5)为流动相,流速1.0 mL·min-1,柱温30℃,检测波长254 nm。结果槲皮苷进样量在0.084 2～0.842μg范围内与峰面积积分值呈良好的线性关系(r=0.999 9),该方法平均回收率为97.8%,RSD为1.2%(n=6)。结论该方法具有简便、准确、重复性好的特点,可用于测定铁扫帚药材中槲皮苷的含量。     

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.

---

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.

     

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.     

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.     

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.