银杏叶中银杏萜内酯的高效液相色谱—电喷雾电离—质谱分析

目的:用高效液相色谱-电喷雾电离-质谱(HPLC-ESI-MS)法对银杏叶中银杏萜内酯进行分析。方法:利用LC-ESI-MS法对银杏叶样品进行了初步研究。液相色谱条件为色谱柱:Inertsil ODS 3,流动相:甲醇-水(36:64),流速1mL·min~(-);质谱为ZMD Micromass电喷雾质谱仪。结果:得到了样品总离子流和选择离子流图,及相应色谱峰的ESI-MS质谱图,对其进行了解析,鉴别出白果内酯及银杏内酯A、B、C、J。结论:本方法快捷、简单和准确。     

不同类型银杏叶中银杏内酯的含量测定

目的 :建立HPLC法测定各种类型银杏叶中银杏内酯的含量。方法 :色谱柱为SUNIERKromasilC1 8(5 μm ,4 6mm×2 5 0mm) ,以 33%甲醇为流动相 ,流速 :1mL·min- 1 ,示差检测器 (RI) ,以银杏内酯A、B、C及白果内酯 4种对照品为对照。结果 :测定了各种类型的银杏叶内酯的含量。结论 :找出了银杏叶的最佳采集时间。     

高效液相色谱-紫外-电喷雾-质谱法分析银杏叶中黄酮醇苷类化合物

目的用高效液相色谱 紫外 电喷雾 质谱 (HPLC UV ESI MS)法对银杏叶中黄酮醇苷类化合物进行分析。方法液相色谱条件为色谱柱 :ZorbaxSBC18( 2 5 0mm× 4 6mm ,5 μm) ;流动相 :异丙醇 四氢呋喃 ( 2 5∶6 5 ) (A)、乙腈 (B)与水 (含甲酸 ,φ =0 5 % ) (C)的三元梯度洗脱 ;检测波长 :35 0nm ;流速 :1mL·min-1;以Agilent多级离子阱质谱仪进行检测。 结果得到了样品紫外色谱图、总离子流色谱图及相应色谱峰的电喷雾 质谱 (ESI MS)一级和二级质谱图。对谱图进行解析 ,鉴别出 12种黄酮醇苷类化合物。结论方法快捷、简便和准确     

银杏叶提取物中银杏内酯A、B、C和白果内酯的提取、分离和结构鉴定

用柱层析结合溶剂法,从银杏叶提取物(EGb)中一次分得银杏内酯A、B、C和白果内酯BB.其结构经IR、1HNMR、13CNMR、MS等波谱确证,纯度经HPLC检测均为单一峰.     

银杏叶提取物中银杏内酯A、B、C和白果内酯的提取、分离和结构鉴定

采用柱层析结合溶剂法,从银杏叶提取物（EGb)中一次分得银杏内酯A、B、C和白果内酯BB。其结构经IR、^1HNMR、^13CNMR、MS等波谱确证,纯度经HPLC检测均为单一峰。     

HPLC-CAD法测定银杏叶片中萜类内酯的含量

目的建立银杏叶片中萜类内酯的含量测定方法。方法采用HPLC-CAD法测定白果内酯、银杏内酯A、银杏内酯B和银杏内酯C的含量。使用Agilent TC C_(18)色谱柱(250 mm×4.6 mm,5μm),以正丙醇-四氢呋喃-水(1∶15∶84)为流动相,流速1.0 mL·min~(-1),柱温40℃,采用电喷雾检测器进行检测。结果各萜类内酯在线性范围内与峰面积线性关系良好,相关系数为0.9997～1.000,平均回收率(n=6)在97.3%～99.1%,RSD在1.6%～2.5%。结论该方法灵敏度高,精密度、重复性、准确度均良好,可作为银杏叶片中萜类内酯的含量测定方法。     

复方雪莲胶囊中大苞雪莲内酯及其β-D-葡萄糖苷和大苞雪莲碱的LC-Q-TOF MS法鉴别

建立了液相色谱-四极杆-飞行时间质谱(LC-Q-TOF MS)法鉴别复方雪莲胶囊中的大苞雪莲内酯及其β-D-葡萄糖苷和大苞雪莲碱.采用Zorbax RRHD C18色谱柱,乙腈-0.1％甲酸为流动相,梯度洗脱.质谱采用电喷雾离子化(ESI)源,以正离子模式采集MS与MS/MS信号.以去氢木香内酯和脯氨酸为参照物,鉴别雪莲花药材和复方雪莲胶囊中的大苞雪莲内酯及其β-D-葡萄糖苷和大苞雪莲碱.     

反相HPLC法测定银杏叶中银杏内酯的含量

目的：测定银杏叶中银杏内酯的含量。方法：实验中采用高效液相色谱（HPLC）测定银杏提取物（GBE）中银杏内酯含量的优化方法,GBE用甲醇溶解后,经酸性氧化铝柱净化,由反向HPLC测定银杏内酯含量。结果：测定银杏内酯含量A,银杏内酯B,银杏内酯C,白果内酯在0.5～7.5μg具有良好的线性关系,平均加样回收率分别为97.2%（相对标准偏差（RSD）为2.4%）、99.3%（RSD=1.9%）、97.4%（RSD=2.5%）。结论：该方法快速、有效,准确度高,重现性好。可用于银杏叶及其提取物（GBE）中银杏内酯的快速测定和分析。     

HPLC-RI法测定银杏叶提取物中4种内酯的含量

目的:建立高效液相色谱法测定银杏叶提取物中4种内酯(银杏内酯 A、银杏内酯 B、银杏内酯 C、白果内酯)的含量。方法:采用 Symmetryshield 型 C_(18)色谱柱(3.9 mm×150 mm,5 μm),以甲醇-水(30:70)为流动相,流速为1.0 mL·min~~(-1),用外标法测定,示差折光检测器检测。结果:4种内酯浓度在0.02～0.24 mg·mL~(-1)范围内,与色谱峰面积呈良好线性关系,相关系数在0.9984～0.9998之间,检测限在0.025～0.035 μg之间,回收率在99.0%～100.2%之间。结论:本方法简单、准确、可靠、灵敏,适用于实验室和企业常规质量控制。     

高效液相色谱蒸发光散射测定银杏叶软胶囊中4种萜类内酯的含量

目的:用HPLC-ELSD测定银杏叶软胶囊中银杏内酯A、B、C及白果内酯的含量.方法:色谱柱填料为十八烷基键合硅胶,流动相为四氢呋喃-甲醇-水(11 : 19:70);漂移管温度为109℃,戴气流速为2.9L·min-1.结果:银杏内酯A、B、C及白果内酯分别在2.994μg～14.970μg、2.967μg～14.835μg、2.955μg～14.775μg5.952μg～29.760μg线性关系良好;银杏内酯A、B、C及白果内酯的平均回收率分别为97.2%、97.5%、97.6%、98.3%.结论:该方法简便、准确、分离效果好;本方法可用于银杏叶软胶囊的质量评价.     

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.