HPLC-CAD法测定浓维磷糖浆中果糖、葡萄糖、蔗糖和麦芽糖含量

目的 建立高效液相色谱串联电喷雾检测器（HPLC - CAD）同时测定浓维磷糖浆中果糖、葡萄 糖、蔗糖和麦芽糖含量的方法,为其质量标准提高提供依据。方法 采用Alltech chrom Prevail carbohydrate ES 5u色谱柱(4.6 mm×250 mm,5 μm),以乙腈-水（75∶25）为流动相,流速 1.0 mL·min^-1,柱温 35 ℃。电喷雾检测器参数为：雾化温度35 ℃,采样频率10 Hz。结果 上述4个糖类成分分离完全,线性关系良好（r均大于0.999 0）;精密度、重复性及回收率实验结果均符合含量测定要求,果糖、葡萄糖、蔗糖和麦芽糖的平均加样回收率分别为98.4%、97.5%、99.4%和95.4%。结论 该方法灵敏度高、准确可靠,可用于于浓维磷糖浆中果糖、葡萄糖、蔗糖和麦芽糖含量测定。     

HPLC示差折光检测法同时测定参芪扶正注射液中单糖和寡糖的含量

目的:建立同时测定参芪扶正注射液中葡萄糖、果糖和蔗糖含量的方法,为中药注射剂糖类成分的测定提供方法和手段。方法:采用高效液相色谱示差折光检测(HPLC-RID)法。色谱柱为Shodex Asahipak NH2P-504E柱,流动相为乙腈-水(75∶25),检测器为示差检测器,流速为1.0mL·min-1,进样量为10μL,柱温为40℃。结果:果糖、葡萄糖和蔗糖进样量分别在19.1～127.3(r=0.9998)、15.9～106.5(r=0.9996)和6.5～43.5μg(r=0.9996)范围内与其峰面积积分值呈良好的线性关系;平均加样回收率分别为97.3%、99.2%和95.6%,RSD分别为4.2%、4.4%、5.2%。结论:该方法操作简便,结果准确可靠,可用于参芪扶正注射液的质量控制,亦可为中药注射剂糖类成分的测定提供方法和手段。     

参麦注射液中糖类成分含量测定研究

目的建立测定参麦注射液中4种糖类成分的反相高效液相色谱法。方法采用Prevail Carbohydrate ES色谱柱(4.6 mm×250 mm,5μm),以乙腈-水(79∶21)为流动相,流速1.0 mL.min-1;ELSD漂移管温度100℃,氮气流速2.8 L.min-1测定果糖、葡萄糖、蔗糖和麦芽糖含量。结果果糖、葡萄糖、蔗糖和麦芽糖分别在0.763 2～15.26 40μg、0.626 8～12.536 0μg、0.860 4～17.208 0μg、0.754 4～15.088 0μg范围内呈良好的对数线性关系。平均回收率分别为99.05%、100.38%、98.75%、99.52%,RSD为1.5%、1.3%、1.7%、1.1%。结论该方法简便、准确、重复性好,可作为参麦注射液的质量控制方法。     

UPLC-ELSD法快速测定生脉注射液中果糖、葡萄糖、蔗糖、麦芽糖含量

目的：建立生脉注射液中主要单糖和双糖含量的快速测定方法。方法：采用超高效液相色谱结合蒸发光散射检测器（UPLC-ELSD）同时测定果糖、葡萄糖、蔗糖、麦芽糖含量。样品经ACQUITYUPLC BEH Amide（2.1 mm×150 mm,1.7 μm）色谱柱分离,柱温35℃。流动相为乙腈（含0.2%三乙胺）-水（75：25）,流速0.2 mL·min^-1。ELSD检测器漂移管温度55℃,氮气压力40.0 psi。结果：4个成分在各自范围内线性关系良好。果糖、葡萄糖、蔗糖、麦芽糖的平均回收率分别为101.6%、99.1%、99.6%、97.9%。生脉注射液中果糖含量最高,3个生产企业的7批样品糖类成分含量差异较大。结论：该方法简便、快速、灵敏、准确,可为中药注射剂的质量控制和物质基础研究提供参考。     

高效液相色谱法测定人乙肝免疫球蛋白中麦芽糖的含量

目的建立高效液相色谱法,测定静脉注射用人乙肝免疫球蛋白(HBIGIV)中麦芽糖的含量.方法采用氨基柱Kromasil 100-5NH2(4.6 mm×250 mm)及示差折光检测器,以0.004 mol·L-1硫酸溶液做流动相,柱温50℃,流速0.8 mL·min-1.结果麦芽糖含量的线性范围5～40 g·L-1,平均回收率(n=6)为99.4%,RSD为1.13%.结论本方法准确、简便,适用于测定人乙肝免疫球蛋白静脉注射液中麦芽糖含量的测定.     

HPLC-CAD法结合化学计量学同时测定甘草中多种糖类

摘要：目的:建立同时测定甘草中多种糖类成分含量的方法。方法:采用高效液相色谱-电喷雾检测器（HPLC-CAD）法,色谱柱为Waters X-Bridge Amide,以乙腈-0.2%三乙胺溶液进行梯度洗脱,流速1.0 ml·min-1,柱温40℃,进样量10μl, CAD氮气压55.0 Pa,雾化器温度35℃,滤光片5.0,采样频率10 Hz。采用化学计量学分析甘草中糖类成分关系,进行模型预测,预判品质优劣。结果:三氯蔗糖、鼠李糖、阿拉伯糖、果糖、甘露糖、葡萄糖、蔗糖、乳果糖、麦芽糖、乳糖、水苏糖分别在各自范围内线性关系良好;精密度、重复性、稳定性RSD均小于3.0%;平均回收率在97.52%～106.28%之间,RSD均小于3.0%（n=6）。与对照药材相比,甘草样品中蔗糖显著偏高,其他糖类成分含量差别不大。相似度、聚类和主成分分析,均得到了一致的结果。结论:该方法操作简便,灵敏度高,适用于甘草中糖类成分的含量测定,结合化学计量学方法,对中药品质鉴定有一定意义。     

高效液相色谱-示差折光检测法测定补中益气丸中蜂蜜的含量

目的建立补中益气丸(蜜丸)蜂蜜中葡萄糖、果糖、蔗糖、麦芽糖含量测定方法,以监控补中益气丸质量。方法 采用高效液相色谱-示差折光检测(HPLC-RD)法;色谱柱为Prevail Carbohydrate ES(250mm×4.6mm,5μm);流动相为乙腈-水(75∶25);流速1.0mL·min-1;柱温:35℃。结果葡萄糖、果糖、蔗糖、麦芽糖对照品分别在17.868～179.14、16.144～161.44、3.016～30.16、6.565～98.475μg线性关系良好,4种成分加样回收率分别为97.1%、101.9%、102.6%、95.9%,RSD分别为0.8%、2.0%、0.8%、1.3%(n=6)。结论该方法操作简便,灵敏度高,重复性好,可用于补中益气丸中蜂蜜的含量测定。     

苦碟子注射液中果糖、葡萄糖和蔗糖的含量测定

目的采用高效液相色谱-蒸发光散射检测法(HPLC-ELSD)测定苦碟子注射液中果糖、葡萄糖和蔗糖的含量。方法采用Prevail Carbohydrate ES糖分析色谱柱(4.6 mm×250 mm,5μm),乙腈(B)-0.1%乙酸水(A)为流动相,线性梯度洗脱,流速为1.0 mL·min-1,柱温为25℃;ELSD检测器:漂移管温度为80℃,雾化气(空气)流速为1.8 L·min-1,测定苦碟子注射液中果糖、葡萄糖和蔗糖含量。结果果糖、葡萄糖和蔗糖在色谱柱上分离效果良好,其平均加样回收率分别为96.7%(RSD=0.70%)、96.6%(RSD=1.3%)、98.6%(RSD=2.9%)。结论该方法简便、稳定、重复性好,可用于苦碟子注射液中果糖、葡萄糖和蔗糖测定,并为其质量控制提供理论依据。     

高效液相色谱法用于蜂蜜的分析及其品质评价

目的：通过测定蜂蜜中果糖,葡萄糖,蔗糖的含量,评价蜂蜜的真伪及质量的优劣,方法：以乙腈－－水（70：30）为流动相,采用高效液相法在糖专用分析柱上测定。结果：品质合格蜂蜜中果糖,葡萄糖含量约为30％,蔗糖含量低于5％,结论：本法可用于天然蜂蜜的品质评价。     

HPLC-ELSD测定红参、麦冬及其制剂中糖的含量

目的 建立同时测定红参、麦冬及其制剂参麦注射液中果糖、葡萄糖、蔗糖、麦芽糖的含量。方法 采用Alltech Prevail Carbohydrate ES(4.6 mm×250 mm,5 μm)色谱柱,流动相为乙腈-水溶液(72∶28),流速：1.0 mL·min^-1,柱温：25 ℃,ELSD氮气压力：3.5 bar,漂移管温度40 ℃。结果 在确定的分析条件下,果糖、葡萄糖、蔗糖、麦芽糖分别在1.01~20.20 mg,0.48~9.66 mg,0.95~19.08 mg,0.96~19.28 μg内呈良好的对数线性关系,回收率均在95%~105%内。结论 该方法简便、准确、稳定,适合用于红参、麦冬及其制剂参麦注射液中各糖的含量测定。     

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.

---

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.