广佛手药材的高效薄层色谱指纹图谱研究

目的 以广佛手药材为基础,建立广佛手挥发油及甲醇提取物的高效薄层色谱(HPTLC)指纹图谱,以评价广佛手药材的质量.方法 应用Merck硅胶GF254高效预制薄层板(20 cm×10 cma),挥发油成分以环己烷-乙酸乙酯-甲酸(8∶2∶0.1)为展开剂展开,5％香草醛硫酸溶液显色;甲醇提取物以环己烷-乙酸乙酯-丙酮-甲酸(6∶2∶3∶0.1)为展开剂展开,10％硫酸乙醇溶液显色;于105℃加热至斑点清晰,分别得广佛手挥发油及甲醇提取物的HPTLC指纹图谱,并用Chromap 1.5软件进行相似度评价及聚类分析.结果 广佛手挥发油的HPTLC指纹图谱由11个特征条斑组成,指认了其中γ-松油烯的条斑;甲醇提取物由8个特征荧光条斑组成,指认了5,7-二甲氧基香豆素的条斑.广佛手不同商品之间挥发油成分及甲醇提取物的差异均较小.结论 HPTLC指纹图谱可为广佛手药材的质量评价提供依据.     

巴戟天不同炮制品的高效薄层色谱指纹图谱研究

目的以巴戟天药材生品为基础,建立巴戟天不同炮制品的高效薄层色谱(HPTLC)指纹图谱,并比较分析生品的指纹图谱。方法硅胶GF254高效预制薄层板,乙酸乙酯部位以石油醚-乙酸乙酯(5∶5.5)为展开剂,上行展开8 cm,10%硫酸乙醇溶液显色;正丁醇部位以正丁醇-冰醋酸-水(4∶1∶5)上层溶液为展开剂,上行展开8 cm,α-萘酚浓硫酸试剂显色。显色后置紫外光灯365 nm或自然光下检视,得薄层色谱指纹图谱,并进行相关分析。结果巴戟天生品的薄层荧光色谱指纹图谱与巴戟肉(蒸制)、盐巴戟天、制巴戟天(甘草制)图谱比较分析,彼此具有明显的区别,可用于生品与巴戟天炮制品的鉴别。结论通过HPTLC指纹图谱考察,生品巴戟天与巴戟肉、盐巴戟天、制巴戟天的区别较大,应分别制定质量评价的标准。     

龙胆泻肝丸（大蜜丸）薄层色谱鉴别方法的建立

目的:对龙胆泻肝丸(大蜜丸)薄层色谱鉴别方法进行研究。方法:采用TLC法,样品用70%甲醇加热回流提取,依次用不同极性的试剂石油醚、乙酸乙酯、正丁醇萃取。石油醚部分化合物,365 nm波长荧光检视,可以检出当归;1%香草醛硫酸显色,可以检出泽泻。乙酸乙酯部分化合物,365 nm波长荧光检视,可以检出黄芩。正丁醇部分化合物,展开剂为三氯甲烷-甲醇-水(30∶12∶3),可以同时检出柴胡和甘草;展开剂为丙酮:乙酸乙酯:水(6∶6∶1),可以检出龙胆苦苷、栀子苷和甘草苷。结果:薄层色谱斑点清晰,分离度好,专属性强,重复性好。结论:本方法可以准确地进行定性鉴别,能够用于龙胆泻肝丸(大蜜丸)的质量控制。     

广藿香不同部位UPLC指纹图谱及化学模式识别研究

目的 建立广藿香药材不同部位的UPLC指纹图谱,研究广藿香不同部位的质量差异。方法 采用UPLC法建立广藿香不同部位化学指纹图谱,结合相似度评价、热图聚类分析（CA）、主成分分析（PCA）及正交偏最小二乘法-判别分析（OPLS-DA）对18批广藿香药材、茎、叶的UPLC指纹图谱进行分析,并测定广藿香酮含量。结果18批广藿香药材及不同部位的UPLC指纹图谱均确定了9个相同的共有峰,并通过对照品指认4、6、9号峰分别为毛蕊花糖苷、异毛蕊花糖苷和广藿香酮。CA和PCA结果表明广藿香叶和茎的质量差异大,叶和药材的质量较接近。OPLS-DA发现5种成分是造成不同批次样品质量差异的主要标志物。含量测定结果表明同一批广藿香中的广藿香酮含量均为茎>药材>叶。结论 广藿香不同部位的化学成分相似,但含量存在显著性差异,本研究可为广藿香药材的质量控制及资源开发利用提供参考。     

消渴康颗粒质量标准研究

目的提高消渴康颗粒的质量标准。方法南五味子鉴别以石油醚(30~60℃)-甲酸乙酯-甲酸(15∶5∶1)为展开剂,在GF254薄层板上展开,254nm下检视;山茱萸鉴别采用硅胶G薄层板,乙酸乙酯-乙醇-冰醋酸(50∶10∶1)为展开剂,50g·L~(-1)香草醛硫酸溶液显色;芒果苷含量测定采用Kromasil C18色谱柱,乙腈-2 mL·L-1冰醋酸溶液(18∶82)为流动相,检测波长258nm,柱温35℃。结果薄层鉴别斑点清晰,阴性对照无干扰;芒果苷在0.021 82~0.218 2μg范围内线性关系良好,回归方程:Y=1 112 484X+1.972 433(r=0.999 9),样品回收率为98.7%,RSD为1.1%。结论该方法简单准确,可用于控制该制剂的质量。     

广藿香挥发油的红外光谱鉴定和气相色谱-质谱分析

目的分析广藿香挥发油的傅里叶变换红外光谱及所含的化学成分。方法采用傅里叶变换红外光谱法和气相色谱-质谱法测定样品挥发油的指纹图谱和化学成分,用色谱峰面积归一法计算各化学成分的相对百分含量。结果从4批广藿香饮片挥发油中共鉴定出20种化学成分,占挥发油总量的90.6%~96.0%。其中特征成分均为广藿香醇(19.6%~46.2%)、广藿香酮(5.2%~27.5%)、α-愈创木烯(3.8%~6.7%)、δ-愈创木烯(4.8%~8.3%)、α-广藿香烯(3.8%~4.3%)、β-广藿香烯(4.5%~14.8%)、刺蕊草烯(4.1%~5.0%)、β-丁香烯(4.3%~5.0%)等。结论上述方法简单,迅速,准确,可用于市售广藿香的质量控制。     

妇炎清颗粒的薄层色谱鉴别

目的用薄层色谱法鉴别妇炎清颗粒中的赤芍、苍术、延胡索、牡丹皮。方法赤芍鉴别以氯仿-乙酸乙酯-甲醇-甲酸（40：5：10：0．2）为展开剂，5％香草醛硫酸溶液为显色荆；苍术的鉴别以石油醚（60-90℃）-乙酸乙酯（20：1）为展开荆，10％硫酸乙醇溶液为显色刺；延胡索的鉴别以正己烷-氯仿-甲醇（7．5：4：1）为展开剂；牡丹皮的鉴别以环己烷-乙酸乙酯（3：1）为展开刺。盐酸酸化的5％三氯化铁乙醇溶液为显色刺。结果各色谱斑点清晰，阴性对照无干扰。结论鉴别方法简便、可靠、灵敏、专属性强，可用于妇炎清颗粒的质量控制。     

中药中48种非法染色色素的TLC法检测

建立了薄层色谱法检测中药中的48种非法染色色素.分别采用乙腈、0.1％甲酸甲醇溶液、甲醇∶0.1％甲酸(3∶2)混合溶液超声提取样品粗粉.将乙腈提取液与脂溶性色素对照溶液点于同一硅胶G板上,以石油醚∶乙醚∶无水甲酸(80∶20∶1)为展开剂展开.将0.1％甲酸甲醇溶液提取液与水溶性碱性色素对照溶液点于同一硅胶G板上,以乙酸乙酯∶乙醇∶水∶氨水(12∶1∶1∶1.2)为展开剂展开.将甲醇∶0.1％甲酸(3∶2)提取液与水溶性酸性色素对照溶液点于同一硅胶G板上,以乙酸乙酯∶乙醇∶水∶氨水(6∶4∶2∶0.2)为展开剂展开.均在日光下检视.48种色素的检测限为0.025～0.6 μg.本法快速简便,可应用于中药材多色素染色初步筛查.     

薄层指纹图谱研究不同断面颜色的土茯苓

目的 建立不同断面颜色土茯苓药材的薄层色谱指纹图谱.方法 高效硅胶G预制板点样1 μL,展开剂为甲苯-乙酸乙酯-甲酸(6∶5∶1.5),饱和20 min,展距8 cm,显色喷以5％三氯化铝乙醇溶液,放置5 min;扫描波长320 nm;狭缝6.0 mm ×0.3 mm,速度20 mm·s-1.结果 红棕色断面样品具有6个共有峰,相似度＞0.95;类白色断面样品具有4个共有峰,相似度＞0.90;在薄层图谱上二者具有显著性差异.结论 所用方法简单且易于操作,专属性强,可用于区分不同断面颜色的土茯苓药材,为区分红棕色断面和类白色断面的土茯苓提供了科学依据.     

薄层色谱法对金黄膏中大黄、黄柏和苍术的鉴别

目的:建立金黄膏中大黄、黄柏和苍术的鉴别方法。方法:采用薄层色谱法,以石油醚(30~60℃)-甲酸乙酯-甲酸(15∶5∶1)的上层溶液为展开剂,鉴别大黄;以甲苯-乙酸乙酯-甲醇-异丙醇-水(6∶3∶2∶1.5∶0.3)为展开剂,鉴别黄柏;以石油醚(60~90℃)为展开剂,鉴别苍术。结果:供试品色谱中斑点的位置及颜色与对照药材及对照品色谱一致。结论:此法可用于金黄膏的定性鉴别。     

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.