陕西产槐角药材不同产地和不同药用部位中槐角苷的含量测定

目的比较陕西产槐角不同产地、不同药用部位(果实、果肉、种子)中槐角苷的含量。方法采用单因素优选槐角提取条件,RP-HPLC法测定,以Thermo C18色谱柱(250mm×4.6mm,5μm)为固定相,甲醇-乙腈-10mL.L-1冰醋酸(40∶5∶55)为流动相;流速:1.0mL.min-1,检测波长:260nm;采用外标法峰面积计算含量。结果槐角在20倍量体积分数65%乙醇下加热回流3次,每次1h,提取的槐角苷含量最高。槐角苷在0.01～0.06mg.mL-1范围内呈良好的线性关系,r=0.999 6,平均加样回收率为98.4%,RSD为2.1%。不同产地槐角药材中槐角苷的含量在7.25%～8.74%之间,以陕西渭南地区的含量最高;不同药用部位果肉中槐角苷含量高于种子。结论该方法操作简便快捷,可作为槐角药材质量的检测手段之一,其结果可为陕西产槐角药材的选材、质量评价以及进一步开发利用提供依据。     

复黄片总鞣质、总黄酮及槐角苷的含量测定

目的建立复黄片中总鞣质、总黄酮及槐角苷的含量测定方法。方法以没食子酸和槐角苷为对照品,UV法测定复黄片中总鞣质及总黄酮的含量,检测波长分别为760和260nm。HPLC法测定复黄片中槐角苷的含量,采用Agilent TC-C18(2)色谱柱(250mm×4.6mm,5μm);柱温为30℃;流动相为乙腈-磷酸缓冲盐,采用梯度洗脱;流速为1.0mL·min-1;检测波长为254nm。结果复黄片中总鞣质、总黄酮及槐角苷的线性范围分别为1.04~5.20(r=0.999 5),4.15~9.34(r=0.999 5)和21.34~74.69μg·mL~(-1)(r=0.999 4),加样回收率分别为99.62%,100.20%和100.70%,平均含量分别为23.81,133.02和9.99mg·片~(-1)。结论该方法简便易行,结果准确、可靠,可用于控制复黄片的质量。     

高效液相色谱法测定槐角中槐角苷的含量

目的:建立HPLC法测定槐角中槐角苷的含量。方法:采用YWG ODS C18柱(250 mm×4.6mm,10μm),以甲醇-乙腈-0.07％磷酸溶液(12:20:68)为流动相,流速为0.9 mL·min-1,紫外检测波长为260 nm。结果:槐角苷在8-120 μg·mL-1的浓度范围内呈良好的线性关系(r=0.9999),平均回收率(n=9)为101.1％,RSD<2.9％。结论:本方法简便、准确,可为评价槐角质量提供依据。     

HPLC测定槐角总黄酮水解产物中的染料木素

目的 采用HPLC测定槐角总黄酮水解产物中染料木素的含量.方法色谱柱为Kromasil C18柱(150 mm×4.6mm,5μm),柱温28℃,流动相为甲醇-水(60∶40),流速1 mL· min-1,榆测波长260 nm.结果染料木素0.02～0.20μg与内峰面积的线性关系良好(r=0.9999),平均回收率为...     

HPLC法测定槐角丸中黄芩苷的含量

目的:建立槐角丸中黄芩苷的含量测定方法.方法:采用HPLC法测定槐角丸中黄芩苷的含量.流动相:甲醇-水-磷酸(45:55:0.2),检测波长:315nm.结果:平均回收率为98.30%RSD=0.84%.结论:本法简便,灵敏,准确,可很好的控制槐角丸的内在质量.     

HPLC-MS/MS法同时测定大鼠血浆中槐角苷及染料木素

目的:建立快速、灵敏的液相色谱-串联质谱方法测定大鼠血浆中槐角苷及其苷元染料木素。方法:血浆经过乙酸乙酯提取,以大豆苷元为内标,采用Zorbax SB-C18(2.1 mm×30 mm,3.5μm)色谱柱,流动相为甲醇-0.001%甲酸铵溶液(加氨水调节pH至7.5)(45∶55),流速0.2 mL·min-1;质谱条件为电喷雾离子源(ESI源),负离子模式检测,扫描方式为多反应监测(MRM),定量离子对为m/z 252.9→223.7(大豆苷元)、m/z 431.1→267.6(槐角苷)、m/z 268.8→132.8(染料木素)。结果:槐角苷浓度在1.072～536 ng·mL-1,染料木素浓度在1.068～534 ng·mL-1的范围内线性关系良好(r>0.995);日间和日内精密度RSD均小于10%,低、中、高3个浓度的提取回收率在85%～97%之间。结论:本法可用于大鼠血浆中槐角苷和染料木素的测定及其药代动力学研究。     

RP-HPLC法测定槐角丸中柚皮苷的含量

目的建立RP-HPLC法同时测定槐角丸中柚皮苷含量的方法。方法色谱柱:ZORBAX SB-C18柱,流动相:甲醇-1%冰醋酸(37.5∶62.5);检测波长283nm;柱温:35℃。结果柚皮苷进样量在0.1012～0.7591μg(r=0.99999)范围内线性关系良好;平均回收率为97.0%,RSD为0.62%。结论该方法简便、快速、准确,适用于槐角丸中柚皮苷的含量测定。     

RP-HPLC法同时测定槐角丸中柚皮苷和黄芩苷的含量

目的:建立RP-HPLC法同时测定槐角丸中柚皮苷和黄芩苷含量的方法.方法:色谱柱:ZORBAX SB-C18柱,流动相:甲醇-1％冰醋酸(37.5:62.5);检测波长280nm;柱温:35℃.结果:柚皮苷、黄芩苷进样量分别在0.1012 ～ 0.7591μg(r=0.99999)、0.2050～1.5378μg(r=0.99999)范围内线性关系良好;平均回收率分别为97.0％、96.4％,RSD分别为0.62％、0.66％.结论:该方法简便、快速、准确,适用于槐角丸中柚皮苷、黄芩苷的含量测定.     

基于HPLC指纹图谱、多指标成分含量测定及化学计量学的槐芩软膏质量评价

目的:建立指纹图谱和多指标定量与化学计量学相结合的槐芩软膏质量评价方法。方法:采用Agilent Extend C₁₈色谱柱(4.6 mm×250 mm, 5μm),柱温25℃,流动相为乙腈-0.2%磷酸水溶液,梯度洗脱,体积流量为1.0 mL·min^-1,检测波长230 nm。利用中药色谱指纹图谱相似度评价软件(2012A版)对10批槐芩软膏建立指纹图谱,确定共有峰并进行相似度评价,并对芍药苷、芦丁、染料木苷、槐角苷、柚皮苷、新橙皮苷、黄芩苷、汉黄芩苷和丹皮酚的含量测定方法进行方法学验证。基于指纹图谱共有峰峰面积测定结果,采用聚类分析和主成分分析等化学计量学方法对不同批次的槐芩软膏进行质量评价。结果:在指纹图谱研究中,标定了21个共有峰,通过与对照品比较指认其中9个色谱峰,并对指认共有峰进行了含量测定。10批槐芩软膏与对照图谱的相似度均在0.90以上。9个成分在各自的质量浓度范围内线性关系良好,平均加样回收率为97.4%～99.2%,RSD为0.86%～1.4%;10批次样品中芍药苷、芦丁、染料木苷、槐角苷、柚皮苷、新橙皮苷、黄芩苷、汉黄芩...     

反相高效液相色谱法测定槐角丸中黄芩苷的含量

目的：用高效液相色谱法测定槐角丸中黄芩苷的含量，以控制该制剂的质量。方法：以C18化学事胶柱分离黄芩苷，以甲醇－水－醋酸（45：55：1）为流动相，以274nm为检测波长进行测定。结果：黄芩苷峰与其它组分峰的分离度为2．9，理论塔板数以黄芩苷峰计算为20180；方法的平均回收率为98．4％（n=5)；5次独立测定的相对偏差为RSD＝0．90％。黄芩苷浓度在0.25-2.5μg范围内，与峰面积呈良好的线性关系。结论：用反相高效液相色谱法测定槐角丸中黄芩苷含量结果准确，重现性好。     

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.