苯磺酸氨氯地平片的HPLC测定

目的建立高效液相色谱法测定苯磺酸氨氯地平片含量,为质量控制提供有效的分析手段。方法色谱柱:Phenom enexODS C18(5μm,4.6 mm×150 mm);流动相:甲醇-0.03 mol.L-1磷酸二氢钾溶液(65∶35);检测波长:239 nm。结果制剂中辅料和有关物质对主药无干扰,苯磺酸氨氯地平在浓度9.952~99.520 mg.L-1范围内线性关系良好,相关系数r=0.9999(n=6);平均回收率分别为99.09%、100.4%、101.2%,RSD为0.12%。结论本法专属性好,准确,简便。     

苯磺酸氨氯地平胶囊的高效液相色谱法测定

目的:建立高效液相色谱法测定苯磺酸氨氯地平胶囊含量,为质量控制提供有效的分析手段.方法:色谱柱:Phenomenex ODS C18( 5μm、4.6mm ×150mm);流动相:甲醇-0.03mol·L-1磷酸二氢钾溶液(65:35);检测波长:2 39nm.结果:制剂中辅料和有关物质对主药无干扰,苯磺酸氨氯地平在浓度9.952～99.520μg·ml-1范围内线性关系良好,相关系数r＝0.9999(n=6);平均回收率分别为99.09%、100.4%、101.2%,RSD为0.12%.结论:本法专属性好,准确,简便.杂质,可有效控制本品质量.     

高效液相色谱法测定雷贝拉唑钠肠溶胶囊的含量和有关物质

目的:采用高效液相色谱法建立雷贝拉唑钠肠溶胶囊有关物质检查及其含量测定方法。方法:Kromasil(4.6mm×250mm,5μm)色谱柱;柱温为20℃:流动相为0.05mol.L-1磷酸二氢钾缓冲溶液(0.1mol.L-1氢氧化钠溶液调pH7.0)-乙腈(70∶30);流速为1mL.min-1;测定波长为290nm。结果:雷贝拉唑钠在50～400mg.L-1范围内线性关系良好,r=0.9998(n=5);平均回收率为99.25%,RSD为2.08%(n=9)。结论:本方法简便,迅速,准确,可靠,专属性强。     

反相高效液相色潽法测定WF-208的含量和有关物质

目的:建立RP-HPLC法测定WF-208的含量并进行有关物质检查。方法:采用Diamonsil C18色谱柱(250 mm×4.6 mm,5μm);流动相:乙腈-甲醇-水(62∶20∶18);流速:1.0 mL.min-1;检测波长:238 nm;柱温:30℃。结果:WF-208在5.00～50.0 mg.L-1范围内线性关系良好(r=0.999 7),平均回收率为99.8%(RSD=0.3%),WF-208与有关物质得到良好的分离,检测限为20μg.L-1。结论:该方法操作简单,重复性好,专属性强,可用于WF-208原料药的含量测定和有关物质的检查。     

RP-HPLC测定盐酸奈必洛尔含量和有关物质

目的建立反相高效液相色谱法测定盐酸奈必洛尔含量和有关物质。方法采用的色谱柱为ODS色谱柱(250 mm×4.6 mm,5μm);以甲醇为溶剂,进样浓度:0.5 g.L-1,0.05 mol.L-1的磷酸盐缓冲液(2%三乙胺,pH=3.5)∶乙腈∶甲醇=200∶115∶40为流动相;检测波长为280 nm。结果盐酸奈必洛尔峰与杂质峰分离良好,盐酸奈必洛尔浓度在31.71～158.55 mg.L-1与峰面积呈良好的线性关系(r=0.999 7),最低检检测限为5 ng。方法精密度RSD为0.35%。结论采用反相高效液相色谱法测定盐酸奈必洛尔含量及其有关物质方法快速简便,结果准确。也可用于该品制剂中有关物质和含量的测定。     

高效液相色谱法测定托拉塞米片中托拉塞米及其有关物质的含量

目的:建立高效液相色谱法测定托拉塞米片中托拉塞米及其有关物质的含量。方法:以岛津ShimpackCLC(M)C18(250mm×4.6mm,5μm)为色谱柱;以甲醇-0.02mol·L-1磷酸二氢钾溶液(用磷酸调节pH至3.0)(65∶35)为流动相;UV检测波长291nm;流速0.9mL·min-1。结果:托拉塞米在2～24mg·L-1范围内具有良好线性关系(r=0.9999),平均加样回收率为99.73%,RSD为0.17%(n=9);3批样品的标示百分含量(%)分别为99.80,100.10,100.40,有关物质的百分含量分别为0.58,0.45,0.39。结论:本方法准确、灵敏,重现性好,可用于托拉塞米片及其有关物质的含量测定。     

高效液相色谱法测定盐酸非索非那定片的含量及其有关物质

目的:建立了高效液相色谱法测定盐酸非索非那定片的含量及其有关物质。方法:色谱柱:DiamonsilC18(200 mm×4.6 mm,5μm);流动相:水(含0.4%磷酸,0.7%三乙胺)-乙腈-甲醇(50∶40∶10),磷酸调pH为3.0;流速:1.0 mL.min-1;检测波长:210 nm;以替米沙坦为内标,计算盐酸非索非那定片的含量。结果:盐酸非索非那定线性范围为1.0~20.0 mg.L-1,r=0.999 8,最低检测限为5μg.L-1,平均回收率为100.5%,3批样品测定平均标示百分含量为93.0%,92.9%,93.8%。结论:本方法简便、准确、专属性强,辅料不干扰主药测定,可用于盐酸非索非那定片的质量控制。     

高效液相色谱法测定吲哚美辛滴眼液含量及有关物质

目的:建立测定吲哚美辛滴眼液中吲哚美辛及其有关物质的方法。方法:采用Hypersil ODS色谱柱(4.6mm×250mm,5μm);流动相:0.1mol.L-1冰醋酸-乙腈(40?60,v/v),检测波长:228nm;柱温:30℃;流速:1.0mL.min-1。结果:制剂中其他成分不干扰测定。吲哚美辛与多种降解产物分离良好。吲哚美辛在24.6~393.6mg.L-1(r=0.999 8,n=6)范围内呈良好的线性关系;模拟回收率平均为100.4%,日内RSD为0.36%(n=5),日间RSD为0.95%(n=5)。结论:该方法简单、快速、准确地测定吲哚美辛的含量及有关物质,可满足吲哚美辛滴眼液的稳定性要求。     

HPLC测定合成胸腺肽α1原料药和有关物质含量

目的研究胸腺肽α1原料含量测定和有关物质考察方法。方法采用反相高效液相色谱法测定,VydacC18色谱柱(250mm×4.6mm,5μm);流动相:0.02mol·L-1磷酸盐缓冲液(pH7.00)-异丙醇(95∶5);柱温:25℃,检测波长:215nm。结果胸腺肽α1线性范围为0.01～0.83mg·mL-1(r=0.9998)。最低检出量为10ng。有关物质含量为2.5%～2.6%。结论该方法简便、可靠、准确,可用于胸腺肽α1含量测定和有关物质考察。     

HPLC法测定盐酸西替利嗪咀嚼片含量及有关物质

目的以高效液相色谱法测定盐酸西替利嗪咀嚼片含量及有关物质。方法采用Luna C18柱(250 mm×4.60 mm,5μm);以甲醇-0.05 mol.L-1乙酸铵溶液(73∶27)为流动相;流量:1.0 ml.min-1;检测波长:230 nm;柱温:室温。结果本方法灵敏、准确、专属行强。线性范围:9.48~56.88 mg.L-1(r=0.9999,n=6);方法回收率为99.78%,RSD=0.53%。结论建立的定量方法专属性强,可以克服辅料对测定的干扰,用于盐酸西替利嗪咀嚼片的质量控制。     

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.