高效液相色谱法测定甘草远志合剂中4种指标成分的含量

目的建立高效液相色谱法同时测定甘草远志合剂中甘草苷、甘草酸铵、3,6'-二芥子酰基蔗糖和细叶远志皂苷的含量。方法采用Kromasil C18色谱柱(4.6 mm×150 mm,5μm),以乙腈为流动相A,以0.1%磷酸溶液为流动相B进行梯度洗脱,流速1.0 mL·min-1,检测波长分别为210、237 nm,柱温30℃。结果甘草苷在10.0¹50.0μg·mL-1(r=0.999 9),甘草酸铵在50150.0μg·mL-1(r=0.999 9),甘草酸铵在50¹ 000μg·mL-1(r=0.999 8),3,6'-二芥子酰基蔗糖在21 000μg·mL-1(r=0.999 8),3,6'-二芥子酰基蔗糖在2⁵0μg·mL-1(r=0.999 7)和细叶远志皂苷在5.050μg·mL-1(r=0.999 7)和细叶远志皂苷在5.0¹30.0μg·mL-1(r=0.999 9)与峰面积呈良好的线性关系,低、中、高3个浓度的平均加样回收率(n=3)均>97%,RSD均<3%,溶液在24 h内稳定。结论本法快速简便、准确可靠、重复性好,可用于测定甘草远志合剂中甘草苷、甘草酸铵、3,6'-二芥子酰基蔗糖和细叶远志皂苷的含量,为甘草远志合剂及其类似制剂的质量评价提供依据。     

HPLC波长切换联合梯度洗脱法同时测定脑灵素胶囊中6个成分的含量

目的建立HPLC波长切换联合梯度洗脱法同时测定脑灵素胶囊中远志?酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、淫羊藿苷、宝藿苷Ⅰ和五味子醇甲的含量。方法采用Spurisil C18色谱柱(250mm×4.6 mm,5μm);流动相为乙腈-0.1%甲酸溶液,梯度洗脱;检测波长分别为320 nm、210 nm、270 nm和250 nm;体积流量为0.9 mL·min-1;柱温为35℃。结果远志?酮Ⅲ、3,6’-二芥子酰基蔗糖、细叶远志皂苷、淫羊藿苷、宝藿苷Ⅰ、五味子醇甲分别在1.18～29.50μg·m L-1(r=0.9996)、3.26～81.50μg·mL-1(r=0.9998)、4.09～102.25μg·mL-1(r=0.9993)、4.66～116.50μg·m L-1(r=0.9999)、2.57～64.25μg·mL-1(r=0.9995)、4.89～122.25μg·mL-1(r=0.9997)内与峰面积线性关系良好,平均回收率分别为97.0%、98.5%、99.2%、98.1%、97.4%和100.0%,RSD分别为1.5%、0.78%、1.2%、1.4%、1.3%和0.66%,10个批次脑灵素胶囊中远志?酮Ⅲ、3,6’-二芥子酰基蔗糖、细叶远志皂苷、淫羊藿苷、宝藿苷Ⅰ和五味子醇甲含量分别为0.237～0.294、0.610～0.753、0.997～1.208、1.099～1.427、0.569～0.728、1.192～1.481 mg·g-1。结论该方法简便、准确、重复性好,可用于脑灵素胶囊中6个成分的同时测定,为脑灵素胶囊的质量评价提供依据。     

HPLC-CAD法测定远志药材中细叶远志皂苷的含量

目的建立高效液相-电雾式检测器(HPLC-CAD)方法测定远志药材中细叶远志皂苷的含量。方法色谱柱为Ultimate XB-C18柱(250mm×4.6mm,5μm);柱温25℃;流动相为甲醇-0.3mL·L~(-1)磷酸溶液(60︰40);流速1mL·min~(-1);进样量10μL;电雾式检测器,雾化温度25℃,采集频率10Hz。结果细叶远志皂苷峰面积与质量浓度线性回归方程:Y=4.295 4 X-0.135 8,r=0.999 9(n=6),线性范围为1.0~10.0mg·mL~(-1);平均回收率为101.4%。结论该方法高效、快速、准确,可作为药物及制剂中细叶远志皂苷的含量测定方法。     

反相高效液相色谱法测定远志中远志皂苷元的含量

目的 :建立反相高效液相色谱法测定远志中远志皂苷元的含量。方法 :采用反相高效液相色谱法。色谱柱为ODS柱(2 5 0mm× 4 6mm ,5 μm) ,流动相为乙腈 -水 - 36 %乙酸 (4 9∶5 1∶0 5 ) ,检测波长为 2 15nm ,流速为 1 0mL·min-1。结果 :线性范围是 42～ 5 2 4μg·mL-1,r =1 0 0 0。理论塔板数为 6 143。测定了我国远志主产区山西 6个产地的远志中远志皂苷元的含量。其含量范围为 1 47%～ 1 5 9%。结论 :本方法灵敏可靠 ,可以用来控制远志的质量。     

HPLC波长切换法同时测定琥珀多寐丸中6个成分的含量

目的建立同时测定琥珀多寐丸中远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B、去氢土莫酸和茯苓酸含量的方法。方法采用波长切换检测的高效液相色谱法,色谱柱采用依利特C_(18)色谱柱,流动相为乙腈(A)-体积分数为0.1%的磷酸溶液(B)系统,进行梯度洗脱;0~36 min检测波长为320 nm(检测远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖),36~75 min检测波长为210 nm(检测细叶远志皂苷、远志皂苷B、去氢土莫酸、茯苓酸);流速为1.3 mL·min~(-1);柱温为30℃。结果在优化的色谱条件下,远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B、去氢土莫酸和茯苓酸分别在6.46~129.20 mg·L~(-1)(r=0.999 2)、6.13~122.60 mg·L~(-1)(r=0.999 5)、13.17~263.40 mg·L~(-1)(r=0.999 9)、14.15~283.00 mg·L~(-1)(r=0.999 6)、5.35~107.00 mg·L~(-1)(r=0.999 7)、4.50~90.00 mg·L~(-1)(r=0.999 3)内浓度与峰面积呈良好的线性关系;6种成分的平均加样回收率(n=6)分别为97.69%、96.87%、100.04%、97.74%、97.67%、99.16%,RSD分别为1.35%、0.96%、0.59%、0.93%、1.02%、1.10%。结论该检测方法可用于琥珀多寐丸中远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B、去氢土莫酸和茯苓酸的含量分析。     

HPLC测定脑灵素胶囊中的远志皂苷元

目的 采用HPLC法测定脑灵素中远志皂苷元的含量.方法 色谱柱为Kromasil C18柱,流动相为乙腈-水(50:50),检测波长为210 nm,流速为1.0 ml·min-1,柱温为30℃.结果 远志皂苷元浓度2.4～90.0 μg·ml-1与峰面积的线性关系良好(r=0.9999),平均加样回收率为96.30%,RSD=2.87%(n=6).结论 所建方法准确、重复性好,可用于测定脑灵素胶囊中的远志皂苷元.     

远志中远志酸的提取分离方法研究

目的 针对现时国内大多数厂家生产的远志制剂中其质量控制标准的远志酸,国外标准品价格昂贵,国内标准品的纯度有待提高的问题,提出从植物远志中提取分离、纯化得到含70.0%以上远志酸的化合物.方法 从植物远志中用95%乙醇回流提取、浓缩得到远志总皂苷,远志总皂苷再经盐酸酸水解,趁热过滤,滤渣用丙酮溶解,用硅胶(100～200目)伴样,干法上柱,过硅胶(100～200目)柱层析,分离得到化合物Ⅰ.根据光谱数据(HPLC、MS)和理化性质等结果 ,可以确定化合物Ⅰ的纯度和结构.结果 化合物Ⅰ纯度约为81.2%的远志酸.结论 (1)从植物远志中分离得到了纯度约为81.2%的远志酸;(2)得到了一种从植物远志中提取分离纯化远志酸的方法 .     

HPLC法测定远志中总皂苷的含量

目的:建立远志药材中总皂苷的含量测定方法。方法:采用远志提取物碱水解方法制备远志总皂苷的次级苷—细叶远志皂苷,采用高效液相色谱法测定细叶远志皂苷的含量。色谱条件为 Alltima C_(18)色谱柱(4.6 mm×250 mm,5 μm),流动相为甲醇0.05%磷酸溶液(65:35),流速1.0 mL·min~(-1),检测波长202 nm。结果:细叶远志皂苷的理论塔板数为2500。回归方程 Y=4.242×10~6X-1.068×10~4(r=0.9999),线性范围100～1000μg·mL~(-1)。平均回收率(n=6)为101.2%(RSD=3.6%)。不同来源14批远志药材含量测定结果表明,远志中含总皂苷以细叶远志皂苷计为2.42%～3.71%;不同采收期样品分析表明,以3～6月份采收含量较高;1～3年生样品分析表明,以2年生和3年生药材含量为高。结论:该方法简便、准确,重复性好,可作为远志药材及含远志复方制剂质量控制方法。建议远志含总皂苷以细叶远志皂苷计应不低于2.5%,采收时间以春季为佳,生长期以2年以上为佳。     

HPLC法测定参茸安神片中远志酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B和五味子醇甲

目的建立HPLC法同时测定参茸安神片中远志酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B和五味子醇甲的方法。方法采用Kromasil C18色谱柱(250 mm×4.6 mm,5μm);流动相:乙腈–0.1%磷酸溶液,梯度洗脱;检测波长:320 nm(0~16 min检测远志酮Ⅲ、3,6'-二芥子酰基蔗糖)、210 nm(16~24 min检测细叶远志皂苷、远志皂苷B)、250 nm(24~35 min检测五味子醇甲);体积流量:1.0 m L/min;柱温:30℃;进样量为10μL。结果远志酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B和五味子醇甲分别在3.85~77.00、6.22~124.40、6.57~131.40、7.61~152.20、4.96~99.20μg/m L线性关系良好(r≥0.999 2);平均回收率分别为98.17%、99.24%、99.90%、97.63%、96.83%,RSD值分别为1.14%、1.23%、0.70%、1.52%、0.81%。结论本法稳定可靠、简便易行,为全面控制参茸安神片的质量提供了参考。     

HPLC法测定穿山龙中伪原薯蓣皂苷、薯蓣皂苷和延龄草苷的含量

目的:建立反相高效液相色谱法同时测定穿山龙中伪原薯蓣皂苷、薯蓣皂苷和延龄草苷的含量。方法:采用Zorbax SB-C18(250 mm×4.6 mm,5μm)色谱柱,流动相为乙腈(A)-水(B),梯度洗脱(0～18 min,25%A线性变为36%A;18～40min,36%A线性变为90%A;40～55 min,90%A保持不变),流速1.0 mL.min-1,检测波长210 nm,柱温30℃。结果:伪原薯蓣皂苷、薯蓣皂苷和延龄草苷的色谱峰面积与浓度呈良好的线性关系,线性范围分别为9.80～588.0μg.mL-1(r=0.9994),20.20～1212μg.mL-1(r=0.9995),5.330～319.8μg.mL-1(r=0.9999);平均回收率(n=9)分别为97.3%,99.4%,97.6%。结论:该方法简便、准确,为穿山龙药材的质量评价提供了方法。     

Synthesis,Cytotoxicity and Antileishmanial Activity of Some N-(2-(indol-3-yl)ethyl)-7-chloroquinolin-4-amines

We report herein the condensation of 4,7-dichloroquinoline (1) with tryptamine (2) and D-tryptophan methyl ester (3) . Hydrolysis of the methyl ester adduct (5) yielded the free acid (6) . The compounds were evaluated in vitro for activity against four different species of Leishmania promastigote forms and for cytotoxic activity against Kb and Vero cells. Compound (5) showed good activity against the Leishmania species tested, while all three compounds displayed moderate activity in both Kb and Vero cells.     

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.

     

Lung disease and PKCs

The lung offers a rich opportunity for development of therapeutic strategies focused on isozymes of protein kinase C (PKCs). PKCs are important in many cellular responses in the lung, and existing therapies for pulmonary disorders are inadequate. The lung poses unique challenges as it interfaces with air and blood, contains a pulmonary and systemic circulation, and consists of many cell types. Key structures are bronchial and pulmonary vessels, branching airways, and distal air sacs defined by alveolar walls containing capillaries and interstitial space. The cellular composition of each vessel, airway, and alveolar wall is heterogeneous. Injurious environmental stimuli signal through PKCs and cause a variety of disorders. Edema formation and pulmonary hypertension (PHTN) result from derangements in endothelial, smooth muscle (SM), and/or adventitial fibroblast cell phenotype. Asthma, chronic obstructive pulmonary disease (COPD), and lung cancer are characterized by distinctive pathological changes in airway epithelial, SM, and mucous-generating cells. Acute and chronic pneumonitis and fibrosis occur in the alveolar space and interstitium with type 2 pneumocytes and interstitial fibroblasts/myofibroblasts playing a prominent role. At each site, inflammatory, immune, and vascular progenitor cells contribute to the injury and repair process. Many strategies have been used to investigate PKCs in lung injury. Isolated organ preparations and whole animal studies are powerful approaches especially when genetically engineered mice are used. More analysis of PKC isozymes in normal and diseased human lung tissue and cells is needed to complement this work. Since opposing or counter-regulatory effects of selected PKCs in the same cell or tissue have been found, it may be desirable to target more than one PKC isozyme and potentially in different directions. Because multiple signaling pathways contribute to the key cellular responses important in lung biology, therapeutic strategies targeting PKCs may be more effective if combined with inhibitors of other pathways for additive or synergistic effect. Mechanisms that regulate PKC activity, including phosphorylation and interaction with isozyme-specific binding proteins, are also potential therapeutic targets. Key isotypes of PKC involved in lung pathophysiology are summarized and current and evolving therapeutic approaches to target them are identified.     

Gender-related symptoms and correlates of alcohol dependence among men and women with a lifetime diagnosis of alcohol use disorders

This study explored gender-related symptoms and correlates of alcohol dependence in a crosssectional study of 150 men and 150 women with a lifetime diagnosis of alcohol use disorders (AUD). Participants were recruited in equal numbers from treatment settings, correctional centres and the general community. Standardized measures were used to determine participants' use of substances, history of psychiatric disorders and psychosocial stress, their sensation seeking and family history of substance use and mental health disorders. Multivariate analyses were used to detect patterns of variables associated with gender and the lifetime severity of AUD. Men had a longer history of severe AUD than women. Women had similar levels of alcohol dependence and medical and psychological sequelae as men, despite 6 fewer years of AUD. More women than men had a history of severe psychosocial stress, severe dependence on other substances and antecedent mental health problems, especially mood and anxiety disorders. There were differences in family history of alcohol-related problems approximating same-gender aggregation. The severity of a lifetime AUD was predicted by its earlier age at onset and the occurrence of other disorders, especially anxiety, among both men and women. The limitations in the generalizability of these findings due to sample idiosyncrasies are discussed.     

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.     

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.