HPLC法同时测定酚氨咖敏颗粒中三组分的含量

目的:建立 HPLC 法同时测定酚氨咖敏颗粒中对乙酰氨基酚、咖啡因、氨基比林的含量。方法:采用日本岛津 VP-ODS色谱柱(150 mm×4.6 mm,5μm),以甲醇-水(40:60)为流动相,流速:1.0 mL·min~(-1),检测波长273 nm,柱温:30℃,进样量:20 μL。结果:对乙酰氨基酚进样浓度在10～100μg·mL~(-1)范围内线性关系良好(r=0.9999),平均回收率(n=3)为98.8%～99.4%;咖啡因进样浓度在2.4～24μg·mL~(-1)范围内线性关系良好(r=0.9999),平均回收率(n=3)为98.2%～101.5%;氨基比林进样浓度在8～80μg·mL~(-1)范围内线性关系良好(r=0.9998),平均回收率(n=3)为98.3%～100.4%。结论:本方法灵敏度高,操作简便、可靠,适用于测定酚氨咖敏颗粒中对乙酰氨基酚、咖啡因、氨基比林的含量。     

HPLC法测定抗菌消炎胶囊中槲皮素和山柰素的含量

目的建立抗菌消炎胶囊中槲皮素和山柰素含量测定的高效液相色谱方法。方法色谱柱:Agilent Eclipse XDB-C18(250mm×4.6mm,5μm);流动相:甲醇-4mL·L~(-1)磷酸溶液(50∶50);柱温:30℃;流速:1.0mL·min~(-1);检测波长:360nm。结果槲皮素质量浓度在1.034~20.68μg·mL~(-1)范围内呈良好的线性关系(r=0.999 3),加样回收率为97.14%,RSD值为0.84%(n=6);山柰素质量浓度在2.061~41.22μg·mL~(-1)范围内呈良好的线性关系(r=0.999 1),加样回收率为98.05%,RSD值为0.59%(n=6)。结论该方法定量准确可靠,操作简便,灵敏度高,可用于抗菌消炎胶囊的质量控制。     

HPLC测定风湿安泰片中马钱子碱和士的宁的含量

目的:采用反相高效液相色谱法测定风湿安泰片中士的宁和马钱子碱的含量。方法:采用 Hypersil BDS C_(18)色谱柱(4.6 mm×250 mm,5 μm),保护柱(4.6 mm×12 mm);乙腈-0.3%三乙胺溶液(磷酸调 pH=2.6)(10:90)为流动相,流速:1.0 mL·min~(-1),柱温:室温,检测波长:254 nm。结果:士的宁在4.6～46μg·mL~(-1)(r=0.9998),马钱子碱在2.65～26.5μg·mL~(-1)(r=0.9998)范围内呈良好的线性关系,士的宁的平均回收率(n=5)为101.1%,RSD 为2.8%;马钱子碱的平均回收率(n=5)为99.6%,RSD 为2.9%。结论:本方法准确、简便、快速,适用于风湿安泰片的质量控制。     

RP—HPLC同时测定菝葜药材中总槲皮素和山柰酚含量

目的:建立同时测定菝葜药材中槲皮素和山柰酚含量的反相高效液相色谱法。方法:色谱柱:Lichrospher C_(18)柱(250 mm×4.6 mm,5 μm),流动相:甲醇-0.5%磷酸水溶液(55:45),流速:1.0 mL·min~(-1),检测波长:365 nm。结果:槲皮素在2.97～29.7μg·mL~(-1)浓度范围内线性关系良好(r=0.9999),山柰酚在3.01—30.1μg·mL~(-1)浓度范围内线性关系良好(r=0.9999),方法回收率分别为98.9%和99.7%。结论:本方法简便、准确,灵敏度高,重复性好,可为评价菝葜药材质量提供依据。     

HPLC法同时测定芩连片中黄芩苷和小檗碱的含量

目的:建立 HPLC 法同时测定芩连片中黄芩苷和小檗碱含量。方法:以芩连片为研究对象,采用 Kromasil ODS(200 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-0.05 mol·L~(-1)磷酸二氢钾溶液-三乙胺(26:74:0.2),流速1.0 mL·min~(-1),检测波长277 nm,柱温为室温。结果:黄芩苷、小檗碱分别在0.0101～0.1217 mg·mL~(-1)(r=0.9997,n=7),0.0114～0.1372 mg·mL~(-1)(r=0.9998,n=7)范围内呈良好线性关系;平均回收率(n=9)分别为98.7%和97.7%。结论:本测定方法简便、快速、准确,为芩连片质量评价提供了依据。     

高效液相色谱法测定苦荞籽壳中芦丁和槲皮素的含量

目的:建立高效液相色谱法测定苦荞籽壳中芦丁和槲皮素的含量。方法:采用 Zorbax SB-C_(18)(4.6 mm×150 mm,5μm)色谱柱;流动相为甲醇-0.4%磷酸(50:50);流速1.0 mL·min~(-1);检测波长254 nm。结果:芦丁进样量在0.024～0.963mg·mL~(-1)范围内(r=0.9996),槲皮素进样量在0.0132～0.528 mg·mL~(-1)范围内(r=0.9990)线性关系良好,平均回收率芦丁为100.1%(RSD=1.15%),槲皮素为99.9%(RSD=1.04%)。结论:该方法操作简便,分离度高,重复性好,可同时测定苦荞籽壳中芦丁和槲皮素的含量。     

新复方大青叶片中4种西药成分的含量测定方法的研究

目的:建立新复方大青叶片中扑热息痛、咖啡因、异戊巴比妥和维生素 C 的含量测定方法。方法:采用 HPLC 法测定了扑热息痛、咖啡因、异戊巴比妥和维生素 C 的含量。结果:扑热息痛在199.5～1247μg·mL~(-1)范围内呈良好的线性关系(r=0.9998),平均回收率为99.81%,RSD=0.99%(n=6);咖啡因在20.64～129μg·mL~(-1)范围内呈良好的线性关系(r=0.9999),平均回收率为100.8%,RSD=1.43%(n=6);异戊巴比妥在8.42～210.5μg·mL~(-1)范围内呈良好的线性关系(r=0.9998),平均回收率为100.4%,RSD=1.41%(n=6);维生素 C 在40.48～253.0μg·mL~(-1)范围内呈良好的线性关系(r=0.9999),平均回收率为99.36%,RSD=1.42%(n=6)。结论:含量测定方法简便准确,重复性好,可用于控制新复方大青叶片的质量。     

RP-HPLC法测定新疆哈萨克族常用药材包尔胡特果实中芦丁和槲皮素的含量

目的建立测定新疆包尔胡特(Rhamnus cathartica L.)果实中芦丁和槲皮素含量的方法。方法色谱柱:依利特Hypersil ODS2C18(260mm×4.6mm,5μm)配预柱;芦丁的流动相:甲醇-10mL·L~(-1)乙酸溶液(70∶30),槲皮素的流动相:甲醇-4mL·L~(-1)磷酸溶液(35∶65);流速均为1.0mL·min~(-1);柱温:30℃;芦丁检测波长:257nm,槲皮素检测波长:360nm;进样量均为10μL。结果芦丁质量浓度在43.411 0~165.600 0μg·mL~(-1)范围内线性关系良好(r=0.999 7),平均加样回收率为99.84%,RSD值为1.45%;槲皮素质量浓度在5.454 0~87.264 0μg·mL~(-1)范围内线性关系良好(r=0.999 9),平均加样回收率为99.83%,RSD值为1.49%。结论该方法简便、准确、重复性好,可用于包尔胡特果实原料中芦丁和槲皮素的含量测定。     

高效液相色谱分离柱后化学发光法同时测定菟丝子中黄酮类成分

目的:建立高效液相色谱分离柱后化学发光法测定菟丝子中芦丁、山柰素、槲皮素和异鼠李素含量。方法:基于在氢氧化钠碱性介质中铁氰化钾可以直接氧化芦丁、山柰素、槲皮素和异鼠李素产生化学发光。色谱柱:Hypersil ODS(5μm,4.6 mm×150 mm),流动相:乙醇-乙腈-水-磷酸(21:22:55:2),流速:1mL·min~(-1),柱温:25℃。结果:芦丁、山柰素、槲皮素和异鼠李素浓度分别在0.2～5μg·mL~(-1)(r=0.9990),0.1～15μg·mL~(-1)(r=0.9991),0.1～100μg·mL~(-1)(r=0.9994),0.3～200μg·mL~(-1)(r=0.9998)范围内,与峰面积有良好的线性关系;检测限(S/N=3)分别为0.02,0.08,0.08,0.03μg·mL~(-1)。结论:水法简便、快速、有效,灵敏度高,首次用于菟丝子中黄酮类成分的测定,取得了很好的结果。     

HPLC测定岩黄连注射液中岩黄连碱的含量

目的:建立 HPLC 法岩黄连注射液中岩黄连碱的含量。方法:Luna C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-水(1:1,1000 mL 含磷酸二氢钾3.4 g,十二烷基硫酸钠1.7g),流速1.0 mL·min~(-1),检测波长347 nm,柱温为室温。结果:岩黄连碱在5.48～49.34μg·mL~(-1)浓度范围内呈良好的线性关系(r=1.0000);方法平均加样回收率为99.96%,RSD=0.41%(n=6)。结论:本法可作为岩黄连注射液的质量控制方法。     

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.     

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.     

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.     

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.