HPLC法测定胆康片中大黄素、大黄酚的含量

目的：建立测定胆康片中大黄素、大黄酚含量的HPLC方法。方法：色谱柱为Waters ODS C18（150mm×4．6mm，5μm），流动相为甲醇-0．1％磷酸溶液（85：15），流速为1．0ml·min^-1，检测波长为254nm。结果：大黄素的线性范围为0．03～0．21μg（r=0．9999）、大黄酚的线性范围为0．06～0．50μg（r=0．9998），大黄素平均回收率为97．9％、RSD为0．2％（n=6），大黄酚平均回收率为97．6％、RSD为0．4％（n=6）。结论：建立的方法简便、重复性好，可用于胆康片中大黄素、大黄酚的含量测定。     

薄层色谱扫描法测定清肾颗粒中蒽醌类衍生物的含量

目的建立同时测定清肾颗粒中蒽醌类衍生物的含量测定方法。方法采用薄层扫描法对清肾颗粒中芦荟大黄素、大黄酸、大黄素、大黄素甲醚、大黄酚进行含量测定。展开剂为正己烷-乙酸乙酯-甲酸(30∶10∶0.5),扫描波长λS=435 nm,参比波长λR=650nm。结果芦荟大黄素的线性范围是0.023 6～0.118 1μg(r=0.998 13),平均回收率101.32%,RSD=2.44%(n=6);大黄酸的线性范围是0.060 0～0.300 0μg(r=0.998 61),平均回收率为101.31%,RSD=1.45%(n=6);大黄素的线性范围是0.045 0～0.225 0μg(r=0.998 41),平均回收率为100.82%,RSD=2.36%(n=6);大黄素甲醚线性范围是0.046 7～0.233 3μg(r=0.99681),平均回收率为100.87%,RSD=2.80%(n=6);大黄酚线性范围是0.032 5～0.162 5μg(r=0.997 56),平均回收率为105.35%,RSD=2.49%(n=6)。结论该方法简便、快捷、准确,可用于清肾颗粒中蒽醌类衍生物的含量测定。     

消炎散质量标准研究

目的 :建立消炎散的质量标准。方法 :采用薄层色谱法对方中大黄、金银花、栀子进行定性鉴别 ;采用高效液相色谱法测定大黄素、大黄酚的含量。结果 :大黄素的线性范围为21 12～105 6ng/ml(r=0.9998 ,n=5) ,平均回收率为98.78 % ;大黄酚的线性范围为29 28～146 4ng/ml(r=0 9998 ,n=5) ,平均回收率为99.45 %。结论 :本方法操作简便、可靠 ,重现性好 ,专属性强 ,可作为消炎散的内在质量控制方法     

HPLC测定菘黄感冒颗粒中大黄酸、大黄素、大黄酚的含量

目的 测定菘黄感冒颗粒剂中大黄酸、大黄素、大黄酚的含量.方法 HPLC,色谱柱为大连依利特ODS 柱(250 mm×4. 6 mm ,5.0 μm),流动相:甲醇∶ 0.1%磷酸溶液(85∶ 15),流速:0.90 ml·min-1, 检测波长:254 nm,柱温:40℃.结果 含量测定大黄酸、大黄素、大黄酚的线性范围分别在3.04～18.24 mg·L-1 (r=0.9999)、6.10～36.60 mg·L-1 (r=0.9999)、8.62～51.72 mg·L-1(r=0.9999),大黄酸平均回收率(n=5)为100.5%(RSD=1.8%),大黄素平均回收率(n=5)为98.35%(RSD=1.9%),大黄酚平均回收率(n=5)为99.25%(RSD=1.5%).结论 建立的含量测定方法简便、快捷、灵敏、准确.     

HPLC法测定壮药驳骨灵酒中大黄素和大黄酚的含量分析

目的建立高效液相色谱法测定驳骨灵酒中大黄素和大黄酚的含量的方法。方法采用Inertsil C18(250×4.6mm,5μm)柱;甲醇-0.1%磷酸溶液(85:15)为流动相;流速:1.0ml/min;检测波长为254nm。结果大黄素线性范围为0.1705～1.364μg(r=0.9997),平均回收率为98.6%,RSD=1.4%(n=6),大黄酚线性范围为0.1008～0.8064μg(r=0.9999),平均回收率为98.9%,RSD=1.4%(n=6)。结论该方法简便,准确,可控制驳骨灵酒中大黄素和大黄酚的含量。     

蒙药益肾散的质量标准研究

目的:建立蒙药益肾散的质量标准。方法:采用薄层色谱法(TLC)对制剂中大黄、诃子进行定性鉴别;采用高效液相色谱法测定制剂中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的含量:色谱柱为Inertsil C18,流动相为甲醇-0.1%磷酸溶液(梯度洗脱),流速为1.0 m L/min,检测波长为254 nm,柱温为35℃,进样量为10μL。结果:大黄、诃子的TLC图斑点清晰,分离度好。芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚检测进样量线性范围分别为23.55~117.75 ng(r=0.999 9)、44.72~223.62 ng(r=0.999 8)、43.18~215.90 ng(r=0.999 7)、77.41~387.12 ng(r=0.999 9)、46.02~230.10 ng(r=0.999 7);精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为95.80%~99.66%(RSD=1.21%,n=6)、95.01%~98.07%(RSD=0.92%,n=6)、95.06%~97.84%(RSD=0.50%,n=6)、95.19%~97.66%(RSD=1.07%,n=6)、95.07%~98.20%(RSD=0.95%,n=6)。结论:该研究所建标准可用于蒙药益肾散的质量控制。     

HPLC法测定舒痔丸中大黄素与大黄酚的含量

目的：建立舒痔丸中大黄素与大黄酚的含量测定方法。方法：采用高效液相色谱法,色谱柱为Phenomenex C18（250mm×4．6mm,5μm）,以甲醇-0．1％磷酸（85：15）为流动相,流速为1．0ml·min^-1,柱温30℃,检测波长为254nm。结果：大黄素和大黄酚线性范围分别在2．46～14．78μg·ml^-1（r=0．9999）和5．33～31．97μg·ml^-1（r=0．9999）;浓度范围内呈良好的线性关系。平均回收率分别为99．13％（RSD=0．99％）和99．64％（RSD=0．27％）（n=6）。结论：本方法简便准确,重复性好,可用于舒痔丸质量控制。     

高效液相色谱法测定星翳明片中丹皮酚含量

目的用高效液相色谱法测定星翳明片中丹皮酚含量。方法采用KromasilC18( 2 0 0mm×4 6mm ,5 μm)色谱柱 ,甲醇 水 (V∶V =5 8∶4 2 )为流动相 ,检测波长 2 74nm ,流速 1 0mL/min。结果线性范围 0 4 896～ 2 4 48μg(r=0 9999,n =5 ) ,平均回收率 99 1 % ,RSD为 1 2 % (n =6)。结论本法适合测定星翳明片中丹皮酚的含量。     

高效液相色谱法测定热毒平胶囊中大黄素及大黄酚的含量

用高效液相色谱法测定热毒平胶囊中大黄素和大黄酚含量结果线性范围分别为大黄素0.075～1.50μg(r=0.9999,n=7)、大黄酚0.106～1.06μg(r=0.9999,n=5),平均回收率分别为大黄素(98.3±1.5)%、大黄酚(101.9±1.2)%.     

RP-HPLC法同时测定抗菌消炎片中7种成分的含量

目的:建立同时测定抗菌消炎片中绿原酸、黄芩苷、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚含量的方法。方法:采用反向高效液相色谱法。色谱柱为Agilent Extend C_(18),流动相为乙腈-0.5%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长分别为327 nm(绿原酸)、280 nm(黄芩苷)和450 nm(芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚),柱温为30℃,进样量为10μL。结果:绿原酸、黄芩苷、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚检测进样量线性范围分别为0.209 4~4.188 0μg(r=0.999 9)、0.372 0~7.440 0μg(r=0.999 9)、0.006 3~0.126 2μg(r=0.999 9)、0.011 6~0.232 2μg(r=0.999 9)、0.005 3~0.106 0μg(r=0.999 8)、0.012 8~0.256 4μg(r=0.999 9)、0.016 5~0.330 3μg(r=0.999 8);定量限分别为2.01、1.93、0.76、1.25、1.24、0.53、1.53 ng,检测限分别为0.98、0.65、0.25、0.42、0.41、0.18、0.52 ng;加样回收率分别为98.41%~100.40%(RSD=0.76%,n=9)、96.17%~100.10%(RSD=1.58%,n=9)、96.11%~100.10%(RSD=1.33%,n=9)、96.29%~100.80%(RSD=1.85%,n=9)、96.88%~100.10%(RSD=1.22%,n=9)、97.81%~101.90%(RSD=1.64%,n=9)、96.46%~101.30%(RSD=1.85%,n=9)。结论:该方法准确可靠,重复性好,可用于抗菌消炎片中7种成分含量的同时测定。     

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.