参芪扶正总苷高效液相色谱指纹图谱

目的 建立参芪扶正总苷的高效液相色谱指纹图谱。方法Waters 717型高效液相色谱仪，Waters 2996二极管阵列检测器，低压四元泵，自动进样器；KR100 5C18色谱柱（250 mm×4.6 mm，5 μm）；流动相为乙腈 水，线性梯度洗脱；柱温：30 ℃；流速：0.8 mL·min-1；检测波长：270 nm；记录时间：90 min。结果10批样品与对照用参芪扶正总苷高效液相色谱指纹图谱的相似度均＞90%，精密度、稳定性、重复性实验中各共有峰相对保留时间和相对峰面积RSD均＜3%。结论该方法操作简便，结果稳定可靠,可作为参芪扶正总苷的质量控制方法。     

槟榔药材C18柱化学特征图谱的研究

摘 要 目的:建立槟榔对照药材的C₁₈柱化学特征图谱和评价指标。方法: 以Inertsil ODS-3 C₁₈(250 mm ×4.6 mm,5 μm）为色谱柱;以甲醇-0.15%三乙胺溶液（磷酸调pH至6.5）（13∶87）为流动相,检测波长为215 nm。结果:供试品特征图谱中呈现3个特征峰,与参照物峰相应的峰为S峰,计算各特征峰与S峰的相对保留时间。相对保留时间规定值：1.10（峰2）、1.63（峰3）。结论:14批样品的相似度均在0.9以上,且方法学考察的结果均符合指纹图谱技术要求。     

尖叶假龙胆薄层色谱特征图谱及高效液相指纹图谱的研究

目的： 建立尖叶假龙胆药材特征图谱及高效液相（HPLC）指纹图谱。方法：采用3种薄层色谱（TLC）法,建立尖叶假龙胆薄层特征图谱。采用HPLC法,建立尖叶假龙胆的指纹图谱,色谱柱为 InertSustain AQ-C18（4.6 mm×250 mm,5 μm）,流动相为甲醇-水,梯度洗脱,流速为1.0 mL﹒min-1,检测波长254 nm,柱温30 ℃,进样量为10 μL。以《中药色谱指纹图谱相似度评价系统（2012A版）》进行相似度评价。结果：所建立的薄层色谱（TLC）法,斑点清晰,分离度良好。建立的尖叶假龙胆药材的HPLC指纹图谱,确定了10 个共有峰,指认了獐牙菜苦苷和龙胆苦苷两个成份,10批不同产地的尖叶假龙胆药材指纹图谱相似度＞0.900,整体相似度较好。结论：所建立TLC鉴别方法和HPLC指纹图谱分析模式,稳定可靠,可为尖叶假龙胆药材的质量控制提供参考。     

芍药总苷高效液相色谱指纹图谱研究芍药总苷高效液相色谱指纹图谱研究

目的研究芍药总苷的高效液相色谱指纹图谱,为科学评价及有效控制其质量提供可靠方法。方法利用HPLC-DAD方法,梯度洗脱,测定了10批芍药总苷样品。色谱条件为:Supelcosil^TM LC-18分析柱(5 μm,150 mm×4.6 mm),柱温25 ℃,流动相A为乙腈;流动相B为水(磷酸调pH为3.0),流动相A梯度洗脱(10%～45%乙腈),分析时间为50 min,时间为0,5,25,27,38,40, 50 min,A(%)为10,15,18,30,35,40, 40％。结果10批芍药总苷样品得到的色谱指纹图谱有22个共有峰,可分为3个部分:保留时间0～5 min处,出现3个小峰;保留时间5～20 min处,有8个峰,其主要特征峰5,6和7均在此区域,通过与标准品的保留时间及紫外光谱比较,5和6号峰分别鉴定为芍药内酯苷和芍药苷;保留时间20～36 min处,有11个峰,另一个主要特征峰12在此区域。最强峰为6号峰,其次为12,5和7,相对峰面积比值为5∶6∶7∶12＝0.267～0.348∶1∶0.108～0.135∶0.405～0.537。相同色谱条件下测定了白芍药材的HPLC图谱,其结果与芍药总苷有很好相关性。结论芍药总苷的指纹图谱特征性及专属性强,可结合含量测定用于全面控制芍药总苷的质量,确保每批产品的均一性。     

咽喉清口含片HPLC特征图谱质量控制方法研究

目的 考察建立咽喉清口含片高效液相色谱（HPLC）特征图谱质量控制方法。方法 采用高效液相色谱法,色谱柱为Waters Symmetry C₁₈柱(4.6 mm×250 mm,5 μm),流动相为乙腈-0.4%磷酸水溶液,梯度洗脱,检测波长为260 nm,流速为1.0 mL·min^-1,柱温为30 ℃,测定10批次咽喉清口含片样品,并将所获得的色谱图导入国家药典委员会颁布的“中药色谱指纹图相似度评价系统（2012版）”,经过多点校正和数据匹配生成色谱特征图谱共有模式,计算各批次样品图谱与标准图谱的相似度,并以色谱图中绿原酸峰为参照峰,计算各色谱峰相对保留时间。结果 得到咽喉清口含片特征图谱共有模式,确认了20个共有特征峰。结论 经过方法学验证,所建立方法稳定可行,可用于咽喉清口含片的质量控制。     

利用高效液相色谱法建立玉屏风总苷的指纹图谱

目的:以黄芪皂苷Ⅱ为参照峰,建立玉屏风总苷HPLC-ELSD的指纹图谱,对玉屏风总苷进行质量控制。方法:采用HPLC-ELSD法,色谱柱为Agilent C₁₈(250 mm×4.6 mm,5 μm);以乙腈和0.1%甲酸为流动相进行梯度洗脱,柱温40℃,流速1.0 ml·min^-1,漂移管温度110℃,N₂载气流速3.30 L·min^-1。结果:建立了玉屏风总苷的HPLC-ELSD的指纹图谱,确定了17个共有峰,并鉴定了其中4个共有峰,各峰相对保留时间的RSD在0.1%~0.75%之间,相对峰面积的RSD在1.68%~4.82%之间。10批总苷样品的相似度均大于0.94。结论:该法简单、精密度、稳定性、重现性好,适用于玉屏风总苷的指纹图谱检测。     

菟丝子HPLC指纹图谱研究

目的优化菟丝子高效液相色谱（HPLC）指纹图谱分析方法,建立菟丝子黄酮类及酚酸类成分指纹图谱。方法采用Zorbax SB C18色谱柱;流动相为乙腈-0.1%磷酸溶液（梯度洗脱）;检测波长为260 nm;柱温为30℃;流速为1.0 mL/min。结果 10批菟丝子样品均标示出13个共有峰,其中9个为黄酮类成分峰,鉴别出4个特征峰（金丝桃苷、异槲皮苷、紫云英苷、山奈酚）;利用中药色谱指纹图谱相似度评价软件进行相似度评价,10批样品的相似度为0.949~0.996,提示菟丝子质量较稳定。结论方法准确可靠,重复性好,为菟丝子质量控制提供了方法依据。     

光皮木瓜特征图谱及3种黄酮类成分含量测定研究

目的 建立光皮木瓜的特征图谱,同时测定芦丁、金丝桃苷、槲皮苷3种黄酮类成分的含量,鉴别光皮木瓜和皱皮木瓜。方法 采用高效液相色谱（HPLC）法。以Agilent 5 TC-C18为色谱柱,以乙腈-0.2%磷酸溶液为流动相进行梯度洗脱,流速为1.0mL/min,柱温为30℃,特征图谱检测波长为330 nm,含量测定检测波长为350 nm。采用《中药色谱指纹图谱相似度评价系统（2012版）》建立光皮木瓜的特征图谱并评价相似度,使用SPSS 23.0软件对15批光皮木瓜（S1～S15）进行聚类分析;测定15批光皮木瓜和7批皱皮木瓜（S16～S22）中3种黄酮类成分的含量,比较二者特征图谱。结果 15批光皮木瓜样品的特征图谱相似度为0.783～0.969;共确定11个特征峰;指认了4种成分,分别为绿原酸、芦丁、金丝桃苷、槲皮苷。15批光皮木瓜样品聚为2类,S5～S8为一类,其余为一类。光皮木瓜与皱皮木瓜的特征图谱有明显区别。15批光皮木瓜样品中芦丁、金丝桃苷、槲皮苷含量分别为48.99～294.45、3.49～102.55、31.98～149.49μg/g,皱皮木瓜中芦丁含量低于光皮木瓜,且皱...     

红景天标准汤剂及配方颗粒高效液相色谱特征图谱研究

目的 建立红景天标准汤剂及配方颗粒的高效液相色谱（HPLC）特征图谱。方法 采用HPLC法,色谱柱为Inert Sustain C18柱（250 mm×4.6 mm,5μm）,流动相为乙腈-0.04%磷酸水溶液（梯度洗脱）,流速为1.0 mL/min,检测波长为278 nm,柱温为30℃,进样量为10μL。以红景天苷为对照,测定15批红景天标准汤剂及小试工艺、中试工艺制成配方颗粒的HPLC图谱,确定共有峰。比较标准汤剂与配方颗粒样品HPLC图谱中共有峰的异同。结果 标准汤剂与配方颗粒样品HPLC特征图谱有5个共有峰,相对保留时间均在规定值的±5%以内。结论 建立的HPLC特征图谱能更好地控制红景天标准汤剂及配方颗粒的质量。     

大接骨丹叶醇提物高效液相色谱指纹图谱研究

目的 建立大接骨丹叶醇提物的高效液相色谱（HPLC）指纹图谱。方法 用70%乙醇提取大接骨丹叶中的成分，采用HPLC法测定，色谱柱为Agela Promosil?C18柱（250 mm×4.6 mm,5μm），流动相为0.2%磷酸溶液-乙腈（梯度洗脱），流速为1.0 mL/min，检测波长为210 nm，柱温为35℃，进样量为10μL。以金丝桃苷为参照峰，绘制10批样品的HPLC指纹图谱，采用中药色谱指纹图谱相似度评价系统2004A版进行相似度评价，确定共有峰，并采用SPSS 18.0统计学软件进行聚类分析和主成分分析。结果 建立了10批样品醇提物的HPLC指纹图谱，确定了11个共有峰，指认了金丝桃苷峰和异槲皮苷峰，10批样品醇提物相似度为0.980～0.999。聚类分析结果显示，10批样品醇提物可聚为2类，其中S1单独聚为一类，S2-S10聚为第二类。主成分分析结果显示，共得到2个主成分，方差贡献率分别为63.533%和23.141%，累计方差贡献率达86.674%。结论 所建立的HPLC指纹图谱及聚类分析和主成分分析方法简便、稳定、可靠、科学，可用于大接骨丹叶醇提物及相关产品的质量...     

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.