Box-Behnken响应面法优化翻白草总黄酮的提取工艺

摘 要 目的：运用Box-Behnken响应面法优化翻白草中总黄酮的提取工艺。方法: 在单因素试验基础上,以提取时间、乙醇浓度以及料液比为考察因素,以翻白草总黄酮提取率为评价指标,利用 Box-Behnken 响应面法优化翻白草中总黄酮的提取工艺。结果: 提取的最佳工艺为：提取浓度为70%的乙醇,每次120 min,液料比为8∶1 ml·g^-1时,黄酮的提取率最高,总黄酮提取率预测值为3.86%,测定值为3.74%,其间相差0.12%。结论:使用Box-Behnken响应面法优化翻白草总黄酮的提取工艺科学可靠,可用于翻白草总黄酮的提取生产。     

Box-Behnken效应面法优化银线草中总黄酮的提取工艺

摘 要 目的： 通过Box Behnken效应面法优化银线草中总黄酮的提取工艺。方法: 以乙醇浓度(X¹)、液料比(X²)和提取时间(X³)为自变量,以银线草中总黄酮的提取量(Y)为因变量,利用Box Behnken效应面法优化银线草中总黄酮的提取工艺。结果: 银线草中总黄酮的最佳提取工艺参数为：乙醇浓度为54.8%,液料比为13.6,提取时间为2.0 h,通过3批验证提取工艺参数,银线草中总黄酮的提取量实测值与回归模型预测值的相对误差为-2.34%。结论:使用Box Behnken效应面法优化银线草中总黄酮的提取工艺,方法简便,精度更高。     

Box-Behnken设计响应面法优选水杨梅总黄酮提取工艺研究

摘 要 目的： 采用Box Behnken设计响应面法优化水杨梅的最佳提取工艺。方法: 以水杨梅中总黄酮含量为评价指标,通过单因素试验分别考察乙醇浓度、液料比、提取时间三个因素对总黄酮含量的影响,采用Box Behnken设计响应面法对水杨梅的提取工艺参数进行优化。结果: 水杨梅的最佳提取工艺：乙醇浓度为 50%,液料比为4.2倍,提取时间为80 min,在该条件下平均提取量12.590 0 mg·g^-1。结论:Box Behnken设计响应面法优化水杨梅总黄酮提取工艺合理,建立的数学模型和试验数据相符,具有较好的预测性。     

响应面设计优化抗癌散总黄酮提取工艺

摘 要 目的： 采用响应面分析法对复方抗癌散总黄酮热回流提取工艺进行优化。方法: 以单因素试验选择了提取时间、乙醇浓度、料液比3个因素为自变量,总黄酮提取率为响应值,通过3因素3水平的响应面分析,确定最佳提取工艺条件。结果: 最佳工艺条件为乙醇浓度64.56%,料液比为1∶26.97,提取时间为2.29 h,提取温度为85℃,总黄酮提取率可达45.94 mg·g^-1。结论: 采用响应面分析法对复方抗癌散总黄酮提取条件优化合理可行,可为其工业生产提供工艺参数依据。     

空心柴胡不同部位中柴胡皂苷a、d和总黄酮的含量比较

摘 要 目的：比较空心柴胡不同部位中柴胡皂苷a、d和总黄酮的含量,为临床合理使用药用部位提供参考。方法: 柴胡皂苷a、d含量测定采用HPLC法：色谱柱Inertsil C18柱（250 mm×4.6 mm,5 μm）;流动相：乙腈-水（40∶60）,流速：1.0 ml·min^-1;检测波长：210 nm,柱温：40 ℃,进样量：10 μl。总黄酮的测定采用比色法：检测波长为500 nm。结果: 柴胡皂苷a、柴胡皂苷d和柴胡总黄酮分别在0.21～1.26 mg·ml^-1(r=0.999 6)、0.25～1.51 mg·ml^-1(r=0.999 7)和4.00～25.00 μg·ml^-1(r=0.999 6)范围内与峰面积呈良好的线性关系;平均回收率分别为99.27%(RSD=2.15%,n=6)、99.4%(RSD=2.14%,n=6)和99.03%(RSD=1.34%,n=6）。空心柴胡根中柴胡皂苷a、d含量分别为0.31%、0.50%,其他部位含量较低;总黄酮在花中含量高达8.48%,在叶、茎、根中依次降低。结论:空心柴胡地上部分富含黄酮类化合物,根中柴胡皂苷含量较高,临床使用带根全草比较合理。     

高效毛细管电泳法测定白术中白术内酯Ⅰ的含量

摘 要 目的： 建立高效毛细管电泳( HPCE) 测定白术中白术内酯Ⅰ（Atractylenolide-1）含量的方法。方法: 运用高效毛细管电泳方法,熔融石英毛细管(75μmID ×50 cm) ,缓冲液为50 mmol·L^-1硼砂缓冲液,检测波长:210 nm ,分离电压:20 kV,柱温25℃,用0.45 μm微孔滤膜过滤后进样,压力进样:50 mbar×5 sec。结果: 方法最低检测浓度为0.5 μg·mL^-1,线性范围2～100 μg·mL^-1,r=0.996,线性关系良好。日内RSD为1.3% ,日间RSD为2.5%,平均回收率分别为97.1%。结论:本法简单、灵敏经济,可作为白术中白术内酯Ⅰ的含量的测定。     

不同炮制方法对麦麸中化学成分的影响

摘 要 目的：分别用高效液相色谱法和紫外可见分光光度法测定湖北麦麸及其炒制品中阿魏酸和总黄酮的含量,探讨不同炮制方法对麦麸中阿魏酸和总黄酮含量的影响。方法: 采用SHIMADZU C18色谱柱（250 mm×4.6 mm,5 μm）,流动相为乙腈 0.1%磷酸水溶液（16∶84）等度洗脱,流速1.0 ml·min^-1,检测波长320 nm,柱温35℃;采用紫外可见分光光度法,在（258±2）nm处对不同炮制品中总黄酮含量进行测定。结果: 麦麸的生品、炒黄品、炒焦品、过焦品、蜜炙品中阿魏酸的含量分别为2.07,2.33,1.68,1.11,0.83 μg·g-1,总黄酮含量分别为5.96,7.15,9.73,13.61,9.42 mg·g-1。结论: 根据麦麸炒制程度的加大,阿魏酸含量呈下降趋势,总黄酮含量呈增加趋势。     

枫蓼肠胃康胶囊中7种黄酮类成分的含量测定及总黄酮提取工艺的优化

摘 要 目的：建立高效液相色谱法同时测定枫蓼肠胃康胶囊中7种黄酮类成分的含量,并对总黄酮提取工艺进行优化。方法: 采用正交试验法优化总黄酮的提取工艺。含量测定色谱条件：色谱柱：Waters RPl8 (250 mm×4.6 mm,5 μm);流动相A：甲醇-水（80∶20）,流动相B：甲醇-0.2%甲酸(17∶83),梯度洗脱;流速：1.0 ml·min^-1;柱温：35℃;可变检测波长(0～27 min,λ1 = 260 nm;27～60 min,λ2 = 360 nm)。结果: 7种黄酮成分在60 min内达到基线分离,线性相关系数均≥0.990 0,平均加标回收率在95.95%～97.84%之间,RSD在0.81%～1.33%之间。总黄酮提取的最佳工艺条件为溶媒倍量1∶15,大孔吸附树脂极性为弱极性（AB-8）,超声提取时间30 min,乙醇体积分数60%。结论:所建立的方法操作简单,精密度高,重复性好,对枫蓼肠胃康胶囊的质量控制和检测都有一定指导意义。     

ASE-HPLC法快速测定决明子中大黄酚和橙黄决明素

摘 要 目的：建立快速溶剂萃取（ASE）及HPLC测定决明子中大黄酚和橙黄决明素的分析方法。方法: 利用正交试验对ASE350快速溶剂萃取系统进行提取方法的研究,采用HPLC法同时测定决明子中大黄酚和橙黄决明素的含量。色谱柱为ACE Excel C18 PFP柱(75 mm×2.1 mm,2.5 μm),流动相为乙腈 0.1%磷酸溶液梯度洗脱,流速为0.4 ml·min^-1,检测波长为284 nm,柱温为40℃。结果: 采用甲醇为萃取溶剂、萃取温度为120℃、静态萃取时间为5 min以及循环萃取3次的方法最优,可以很好地提取决明子中大黄酚和橙黄决明素,耗时仅为药典提取方法的1/9。大黄酚和橙黄决明素线性范围为0.73~58.57 μg·ml^-1(r=0.999 7)和1.09~87.29 μg·ml^-1（r=0.999 6),平均回收率分别为102.7%（RSD=0.8%）和98.2%（RSD=1.5%）。 结论:该方法能简便、快速、准确的测定决明子中的大黄酚和橙黄决明素。     

HPLC法测定甲磺酸沙芬酰胺中对映异构体的含量

摘 要 目的： 建立测定甲磺酸沙芬酰胺中对映异构体含量的方法。方法: 采用HPLC法,色谱柱： Chiralpak AS-H柱（250 mm×4.6 mm,5 μm）;流动相：正己烷-乙醇-二乙胺（75∶25∶0.1）;流速：1.0 ml·min^-1;检测波长：225 nm;柱温：35℃。结果: 甲磺酸沙芬酰胺与其对映异构体之间的分离度大于2.0;两者分别在1.007~2517.500 μg·mL^-1和0.909~2273.200 μg·mL^-1范围内呈良好的线性关系,r均为0.999 0;对映异构体的平均加样回收率为104.9%,RSD为2.3%（n=9）。结论:该方法准确、快速,可用于甲磺酸沙芬酰胺产品中对映异构体的含量测定。     

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.