反相高效液相色谱法测定塞克硝唑的含量及其有关物质

目的采用反相高效液相色谱法测定塞克硝唑的含量及其有关物质.方法采用Inertsil ODS C18色谱柱(5μm,4.6 mm×150 mm),以乙腈-水(10∶90)为流动相,流速1.5 mL*min-1,检测波长320nm.结果反相高效液相色谱法测定的线性范围为0.5～700.0μg*mL-1,相关系数r=0.9999;日内精密度为0.38%(n=6),日间精密度为0.44%(n=6).结论采用反相高效液相色谱法测定塞克硝唑的含量及有关物质,方法简便、快速、准确、专属性好.     

RP-HPLC法测定接骨木中盐酸小檗碱的含量研究

目的采用反相高效液相色谱法建立接骨木中盐酸小檗碱含量的测定方法。方法采用反相高效液相色谱法,色谱柱:Hypersil ODS C18(4.6 mm×250 mm,5μm);流动相:甲醇-水-磷酸(25∶75∶0.2);柱温:30℃;检测波长:340 nm。结果盐酸小檗碱在4.90⁴9.0μg·mL-1范围内线性关系良好(r=0.999 8),精密度试验的RSD=0.36%,样品稳定性试验的RSD=1.08%,样品重复性试验的RSD=0.92%,平均回收率为98.68%(RSD=0.55%)。结论反相高效液相色谱法测定接骨木中盐酸小檗碱含量的方法简单、准确度高、重现性好,为制定接骨木的质量控制标准提供参考依据。     

高效液相色谱法测定布洛芬混悬液中布洛芬含量

目的:用高效液相色谱法测定布洛芬混悬液中布洛芬的含量。方法:采用Symetry C18柱(3.9mm×150mm,5μm)为分析柱,乙腈∶醋酸-醋酸钠缓冲液(60∶40)为流动相,流速1.0mL.min-1,检测波长263nm:,柱温40℃。结果:布洛芬在40~120μg.min-1范围内浓度与峰面积线性关系良好,回归方程为A=643.49C 11 229(r=0.997 2),日内和日间精密度RSD<2%。结论:高效液相色谱法简便、准确,可用于布洛芬混悬液的质量控制。     

氟康唑氯化钠注射液中氟康唑及有关物质的含量测定

目的:建立用高效液相色谱法(HPLC法)测定氟康唑氯化钠注射液中氟康唑及有关物质含量的方法。方法:色谱柱为ShimadzuVP-ODS柱(150mm×4.6mm,5μm),流动相为pH=7.0的磷酸缓冲溶液-甲醇(55∶45),流速为1mL/min,检测波长为261nm。结果:氟康唑浓度在20.6～72.1μg/mL范围内与峰面积呈良好线性关系,r=0.9992,精密度试验的RSD为0.59%(n=6),最低检测限为4×10-2μg,平均回收率为99.61%,RSD为0.3%。结论:该法准确,精密度高,重现性好,可作为氟康唑氯化钠注射液的含量测定和有关物质检查方法。     

反相高效液相色谱法测定石菖蒲挥发油β-细辛醚血药浓度

目的:建立反相高效液相色谱法测定石菖蒲挥发油β-细辛醚在大鼠血清中的药物浓度.方法:血清样品用甲醇提取及沉淀蛋白.色谱柱为Hypersil Division ODS C18柱(150mm×4.6mm,5μm);流动相为甲醇-水(60∶40),1 000mL流动相中加入磷酸二氢钾1.4g和十二烷基磺酸钠1.2g;流速为1.0mL*min-1,室温操作,检测波长为257nm.结果:该方法回收率为95.74%～102.27%,RSD<7.0%,在大鼠血清中最低检测浓度为0.01μg*mL-1.血清中β-细辛醚浓度在0.056～4.536μg*mL-1范围内线性关系良好(r=0.999 6).结论:方法快速准确,样品处理简便易行,适于石菖蒲挥发油β-细辛醚血药浓度测定及药动学研究.     

RP-HPLC测定血清中氧氟沙星的浓度

目的建立测定血清中氧氟沙星浓度的方法。方法采用反相液相色谱-荧光法。固定相为Phenomenex C18柱(5μm,4.6 mm×250 mm);流动相为甲醇-0.05 mol.L-1磷酸二氢钠溶液p、H2.3(35∶65);检测波长λex=298 nm,λem=491 nm;流速1.0ml.min-1。结果氧氟沙星的线性范围为0.037~4.064μg.ml-1(r=0.9997);方法回收率及提取回收率分别为97.3%和92.4%;其日内精密度RSD<3.2%,日间精密度RSD<5.4%。结论所用方法准确、简便、重复性好,适用于生物样品中氧氟沙星的浓度测定。     

RP—HPLC法测定羧胺三唑含量及有关物质

目的:采用反相高效液相色谱法测定羧胺三唑的含量及其有关物质。方法:采用Kromasil C_(18)色谱柱(4.6mm×250mm,5μm);以乙腈-水相(45∶55)为流动相;流速2.0mL·min~(-1);检测波长:262nm;柱温:室温;进样量:20μL。结果:反相高效液相色谱法测定的线性范围为12.5～200μg·mL~(-1);相关系数r=0.9999;日内精密度:RSD为0.38%(n=5);日间精密度:RSD为0.39%(n=5)。结论:本法简便快速、准确、专属性好。     

离子对色谱法测定复方西吡氯铵含片中维生素C及有关物质

目的:采用反相离子对高效液相色谱法测定复方西吡氯铵含片中维生素C及有关物质.方法:采用Shimadzu CLC-ODS柱(150mm×6.0mm,5μm),以甲醇-水(含0.005mol*L-1十六烷基三甲基溴化铵和0.050mol*L-1磷酸二氢钾)(10∶90)为流动相,流速为1.0mL*min-1,检测波长为254nm.结果:离子对高效液相色谱法测定的线性范围为5.0～200μg*mL-1,相关系数r=0.999 9;日内精密度为0.52%(n=6),日间精密度为0.86%(n=6);平均回收率为99.54%(n=9).结论:采用反相离子对高效液相色谱法测定复方西吡氯铵含片中维生素C的含量及其有关物质,方法简便、快速、准确、专属性好.     

高效液相色谱法测定盐酸伪麻黄碱的血药浓度

目的:建立反相高效液相色谱法测定伪麻黄碱的血药浓度方法。方法:采用Zorbax SB-C18柱(4.6mm×250mm,5μm),流动相:0.2%磷酸溶液-乙腈(95∶5),流速:1.0mL.min-1,检测波长为194nm。结果:线性范围50~1 000μg.L-1(r=0.999 3),平均回收率79.20%。日内、日间RSD<5%,最低定量浓度为25μg.L-1。结论:该法简便、快速、准确,适用于伪麻黄碱药动学和生物等效性研究。     

反相高效液相色谱法测定人血清中万古霉素的浓度

目的 建立反相高效液相色谱法测定人血清中万古霉素(糖肽类抗菌药)的浓度.方法 色谱柱为Shimadzu Shim-pack VP-ODS柱,流动相为甲醇-乙腈-0.05 mol·L-1磷酸二氢钾缓冲液(pH 3.2)=6.5:8.5:85,流量0.8 mL·min-1,紫外检测波长236 nm;盐酸去甲万古霉素为内标.结果 血清万古霉素在1-100 mg·L-1内线性良好,回归方程Y=24.09x-0.08(n=7,y=0.9993),日内和日间精密度RSD<10%.结论 该测定方法可靠,可用于临床血清万古霉素的浓度监测.     

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.     

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.     

Biochemical and molecular characterisation of cubozoan protein toxins

Class Cubozoa includes several species of box jellyfish that are harmful to humans. The venoms of box jellyfish are stored and discharged by nematocysts and contain a variety of bioactive proteins that are cytolytic, cytotoxic, inflammatory or lethal. Although cubozoan venoms generally share similar biological activities, the diverse range and severity of effects caused by different species indicate that their venoms vary in protein composition, activity and potency. To date, few individual venom proteins have been thoroughly characterised, however, accumulating evidence suggests that cubozoan jellyfish produce at least one group of homologous bioactive proteins that are labile, basic, haemolytic and similar in molecular mass (42-46 kDa). The novel box jellyfish toxins are also potentially lethal and the cause of cutaneous pain, inflammation and necrosis, similar to that observed in envenomed humans. Secondary structure analysis and remote protein homology predictions suggest that the box jellyfish toxins may act as α-pore-forming toxins. However, more research is required to elucidate their structures and investigate their mechanism(s) of action. The biological, biochemical and molecular characteristics of cubozoan venoms and their bioactive protein components are reviewed, with particular focus on cubozoan cytolysins and the newly emerging family of box jellyfish toxins.     

Dose tolerability of chronically inhaled voriconazole solution in rodents

Invasive pulmonary aspergillosis (IPA) is a fungal disease of the lung associated with high mortality rates in immunosuppressed patients despite treatment. Targeted drug delivery of aqueous voriconazole solutions has been shown in previous studies to produce high tissue and plasma drug concentrations as well as improved survival in a murine model of IPA. In the present study, rats were exposed to 20 min nebulizations of normal saline (control group) or aerosolized aqueous solutions of voriconazole at 15.625 mg (low dose group) or 31.25 mg (high dose group). Peak voriconazole concentrations in rat lung tissue and plasma after 3 days of twice daily dosing in the high dose group were 0.85 ± 0.63 μg/g wet lung weight and 0.58 ± 0.30 μg/mL, with low dose group lung and plasma concentrations of 0.38 ± 0.01 μg/g wet lung weight and 0.09 ± 0.06 μg/mL, respectively. Trough plasma concentrations were low but demonstrated some drug accumulation over 21 days of inhaled voriconazole administered twice daily. Following multiple inhaled doses, statistically significant but clinically irrelevant abnormalities in laboratory values were observed. Histopathology also revealed an increase in the number of alveolar macrophages but without inflammation or ulceration of the airway, interstitial changes, or edema. Inhaled voriconazole was well tolerated in a rat model of drug inhalation.