HPLC法测定复方金刚烷胺氨基比林片中氨基比林的含量

目的:建立HPLC法测定复方金刚烷胺氨基比林片中氨基比林的含量.方法:色谱柱为Agilent C18(250 mm×4.6mm,5μm),流动相为甲醇-1%醋酸溶液(用二乙胺调节pH至3.7)(34:66),流速1.0 ml·min-1,检测波长为260 nm.结果:氨基比林在18.7～32.1μg·ml-1范围内呈良好的线性关系(r=0.999 8),平均回收率99.7%,RSD0.3%(n-5).结论:方法专属性强,可用于复方金刚烷胺氨基比林片氨基比林的含量测定.     

HPLC法同时测定复方金刚烷胺氨基比林片中氨基比林和马来酸氯苯那敏的含量及含量均匀度

目的:建立同时测定复方金刚烷胺氨基比林片中氨基比林和马来酸氯苯那敏含量的高效液相色谱(HPLC)法,并考察马来酸氯苯那敏的含量均匀度。方法:色谱柱采用XBridge C 18柱(4.6 mm×250 mm,5μm),流动相为0.05 mol·L^-1磷酸二氢钠-乙腈(80∶20)(用磷酸调pH值至2.5),流速为1.0 mL·min^-1,柱温为40℃,检测波长为262 nm,进样量为20μL。结果:复方金刚烷胺氨基比林片中的氨基比林和马来酸氯苯那敏的分离度均符合要求,质量浓度线性范围分别为36~96μg·mL^-1(r=0.9999),12~32μg·mL^-1(r=0.9998);平均加样回收率分别为99.92%、100.70%,RSD分别为0.89%、0.84%(n=9)。按拟定的方法,分别对3个批次的样品进行含量测定,计算含量,氨基比林的含量分别为104.4%、104.2%、99.5%;马来酸氯苯那敏的含量分别为98.8%、102.8%、101.5%。结论:该方法简便、快捷、准确,适用于复方金刚烷胺氨基比林片中氨基比林和马来酸氯苯那敏的含量测定以及马来酸氯苯那敏含量均匀度的测定,有利于质量控制。     

HPLC法测定复方金刚烷胺氨基比林片中氨基比林的溶出度

目的建立一种用高效液相色谱法测定复方金刚烷胺氨基比林片中氨基比林溶出度的方法。方法以水为溶出介质,转速为100 r.min-1,30 min时取样。选用色谱柱SunfireC18(250 mm×4.6 mm,5μm);流动相为甲醇-水(56:44);检测波长:273 nm;流速:1.0 mL/min。结果氨基比林在11.9～71.47μg/mL浓度范围内与峰面积呈良好的线性关系(r=0.9999)。平均回收率为99.05%。结论本方法简单、快速、结果准确可靠。     

HPLC-ELSD法测定复方金刚烷胺氨基比林片中氨基比林和盐酸金刚烷胺的含量

摘 要 目的：建立一种测定复方金刚烷胺氨基比林片中氨基比林和盐酸金刚烷胺含量的HPLC ELSD法。方法: 色谱柱：Aglient Eclipse Plus C18 柱（250 mm×4.6 mm,5 μm）;流动相：0.1%的三氟醋酸溶液 乙腈(85∶15);流速：0.7 ml·min^-1;柱温：室温;蒸发温度：40℃;雾化温度：40℃;载气（氮气）流速：1.8 L·min^-1,进样量：10 μl。结果: 氨基比林和盐酸金刚烷胺分别在606.72～3 033.60 μg·ml^-1、400.96～2 004.80 μg·ml^-1范围内峰面积与进样量的对数呈现良好的线性关系（r分别为0.999 7、0.999 4）;平均回收率分别为99.5%、99.3%,RSD分别为0.35%、0.40%（n=9）。结论:该方法简便、快速、准确、重复性好,适用于复方金刚烷胺氨基比林片中氨基比林和盐酸金刚烷胺的含量测定。     

HPLC法测定复方氨林巴比妥注射液中氨基比林和安替比林的含量

目的:建立测定复方氨林巴比妥注射液中氨基比林和安替比林含量的方法。方法:采用Phenomenex C18色谱柱(250 mm×4.6 mm,5μm),以甲醇-水(45∶55)为流动相,检测波长285 nm,流速0.8 ml/min,柱温40℃。结果:氨基比林的线性范围为0.125~0.437 mg/ml(r=0.999 9),平均回收率为99.0%(n=6),安替比林的线性范围为0.050~0.176 mg/ml(r=0.999 9),平均回收率为101.1%(n=6)。结论:本方法简便快速,结果准确,重现性好,适用于复方氨林巴比妥注射液的含量测定。     

HPLC法测定复方金刚烷胺氨基比林片中马来酸氯苯那敏的含量及含量均匀度

目的：建立用HPLC法测定复方金刚烷胺氨基比林片中马来酸氯苯那敏的含量及含量均匀度。方法：色谱柱为DiamonsilC18柱（250mm×4．6mm,5μm）,流动相为0．0015％庚烷磺酸钠溶液（含三乙胺0．08％,用冰醋酸调pH至3．3）-甲醇-乙腈（31：47：22）,检测波长为262nm,流速为1．0ml·min^-1。结果：线性范围为0．10～0．70μg（r=0．9998）,平均回收率为100．4％,RSD为0．5％（n=6）。结论：方法简便准确、灵敏度高,重复性好,可用于复方金刚烷胺氨基比林片中马来酸氯苯那敏的含量及含量均匀度测定。     

HPLC测定复方氨基比林注射液中氨基比林,安替比林,巴比妥含量

目的:探讨用HPLC法测定氨基比林注射液中氨基比林、安替比林、巴比妥含量的方法。方法;在μBondpark C;柱上,以乙腈-水-三乙胺-乙酸为流动相,于211nm波长处检测。结果:平均回收率,氨基比林为100.93％(n=5),RSD=0.5％;安替比林为100.47％(n=5),RSD=0.8％;巴比妥为100.6％(n=5),RSD=0.6％。结论:本方法简便、快速、准确、重视性好,适用于该品种生产过程中的质量控制。     

高效液相色谱法测定氨咖甘片中咖啡因及氨基比林的含量和溶出度

目的:建立同时测定氨咖甘片中咖啡因及氨基比林的含量和溶出度的高效液相色谱分析方法.方法:采用ODS色谱柱(150 mm×4.6 mm,5μm),流动相为甲醇-水(45:55),检测波长285 nm,流速:1.0 mL·min-1.采用外标法分别测定咖啡因和氨基比林的含量及溶出度.结果:标准曲线的线性范围为咖啡因0.01～0.20 g·L-1,氨基比林0.06～0.95 g·L-1.加样回收率咖啡因为99.5%～100.7%,氨基比林为98.4%～100.0%.结论:本方法快速、可靠、简单、灵敏,适用于该制剂的质量分析检验.     

HPLC法测定氨酚比林注射液中对乙酰氨基酚和氨基比林的含量

目的:建立氨酚比林注射液中对乙酰氨基酚、氨基比林含量的高效液相色谱方法。方法:选用AgilentSBC18(150 mm ×4．6mm,5μm),乙腈-0．1％磷酸溶液-三乙胺(12:87:1)为流动相,检测波长为240 nm,流速为1．0 ml·min-1。结果:对乙酰氨基酚的线性范围为0．35-1．74μg(r=0．999 9),平均回收率为101．4％,RSD=0．5％;氨基比林的线性范围为0．48～2．42 μg,r=0．999 9,平均回收率为100．3％,RSD=0．4％。结论:本方法快速、准确,样品处理简便易行。     

改变波长高效液相色谱法测定氨咖敏片中氨基比林和咖啡因含量

目的建立改变检测波长的高效液相色谱(HPLC)法,测定氨咖敏片的氨基比林和咖啡因含量。方法采用Agilent C18柱(150 mm×4.6 mm,5μm),以甲醇-水-冰醋酸(40:60:0.2)为流动相,流速为1.0 mL/min,进样量为20μL,检测温度为室温,检测波长0～3 min时为263 nm,3～15 min时为273 nm。结果氨基比林的平均回收率为99.2%,RSD=0.28%(n=6);咖啡因的平均回收率为98.2%,RSD=0.41%(n=6)。结论该方法简单、可靠。     

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.