高效液相色谱法同时测定双黄消炎片中黄芩苷和黄芩素含量

目的 建立同时测定双黄消炎片中黄芩苷和黄芩素含量的反相高效液相色谱法.方法 色谱柱采用Agilent Eclipse XDB-C18柱(250 mm ×4.6 mm,5μm),以甲醇-0.1%磷酸溶液为流动相(梯度洗脱),检测波长为277 nm,流速1.0 mL/min,进样量10μL,柱温35℃.结果 黄芩苷质量浓度在5.678~141.95μg/mL范围内与峰面积有良好线性关系,r=1.000 0(n=7);黄芩素质量浓度在2.122~53.05 μg/mL范围内与峰面积有良好线性关系,r=1.000 0(n=7).黄芩苷平均回收率为99.32%,RSD为0.63%(n=6);黄芩素平均回收率为99.27%,RSD为0.48%(n=6).结论该法操作简便、快速、结果准确,可用于双黄消炎片的质量控制.     

HPLC法同时测定双黄消炎片中黄芩苷、药根碱、巴马汀及小檗碱的含量

目的:用 HPLC 法同时测定双黄消炎片中黄芩苷和3种生物碱类成分药根碱、巴马汀及小檗碱的含量。方法:色谱柱:Diamonsil~(TM)(钻石)C_(18)柱(250 mm×4.6 mm,5μm);流动相:0.1%磷酸(加三乙胺调 pH 至2.97)-乙腈(75:25);流速:1.0 mL·min~(-1);检测波长:345 nm。结果:黄芩苷、药根碱、巴马汀和小檗碱分别在0.13～2.7μg(r=0.9998),0.0097～0.19μg(r=0.9998),0.010～0.20μg(r=0.9999),0.020～0.40μg(r=0.9998)范围内线性关系良好;4个成分的平均回收率(n=9)分别为100.4%,99.7%,100.1%,100.4%。结论:本方法快速、简便,重复性好,可作为该制剂的质量控制方法。     

HPLC法测定七制香附丸中芍药苷和黄芩苷的含量

目的建立高效液相色谱法测定七制香附丸中芍药苷和黄芩苷的含量。方法色谱柱为Capcell PAK C18柱(4.6 mm×250 mm,5μm),流动相组成A:乙腈,B:0.2%磷酸水溶液,梯度洗脱,检测波长为230 nm(0⁵min,80%B;55min,80%B;5¹5 min,80%B→50%);280 nm(1515 min,80%B→50%);280 nm(15²2 min,50%B→20%;2222 min,50%B→20%;22²6 min,20%B);流速:1.0 mL·min-1,柱温:30℃。结果芍药苷和黄芩苷线性关系良好,线性范围分别为0.4026 min,20%B);流速:1.0 mL·min-1,柱温:30℃。结果芍药苷和黄芩苷线性关系良好,线性范围分别为0.40⁴.76μg,0.664.76μg,0.66⁷.97μg,平均回收率(n=6)分别为98.42%(RSD=0.83%),99.10%(RSD=1.16%)。结论本方法操作简便,结果准确,重复性好,可用于测定七制香附丸中芍药苷和黄芩苷的含量。     

HPLC法同时测定舒肝宁注射液中5种成分的含量

目的:建立同时测定舒肝宁注射液中5种成分含量的方法。方法:采用高效液相色谱法。色谱柱为Symmetry~? C_(18),流动相为甲醇-0.4%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为238 nm(栀子苷、黄芩苷)、327 nm(绿原酸、野黄芩苷、黄芩素),柱温为30℃,进样量为10μL。结果:绿原酸、栀子苷、黄芩苷、黄芩素、野黄芩苷检测质量浓度线性范围分别为0.406 2~26.0μg/mL(r=0.999 9)、2.500 0~160.0μg/mL(r=0.999 9)、6.562 0~420.0μg/mL(r=0.999 9)、0.312 5~20.0μg/mL(r=0.9996)、0.585 9~37.5μg/mL(r=0.999 8);定量限≤31.20 ng,检测限≤15.60 ng;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为97.72%~101.10%(RSD=1.21%,n=6)、97.67%~102.40%(RSD=1.87%,n=6)、97.64%~101.10%(RSD=1.31%,n=6)、96.45%~100.10%(RSD=1.47%,n=6)、96.16%~101.10%(RSD=1.69%,n=6)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于舒肝宁注射液中5种成分含量的同时测定。     

高效液相色谱法测定双黄口服液中芍药苷和黄芩苷含量

目的建立测定双黄口服液中芍药苷和黄芩苷含量的高效液相色谱法。方法色谱柱为Ultimate XB-C18柱（250mm×4.6mm,5μm）,流动相为甲醇-水-醋酸（35：65：1）,流速1.0mL/min,检测波长244nm。结果芍药苷和黄芩苷质量浓度均在25～250μg/mL范围内与峰面积线性关系良好,相关系数分别为0.9997和1.0000,平均回收率分别为97.74%和97.06%（n=6）。结论所用方法可同时测定双黄口服液中芍药苷和黄芩苷的含量,且方法简便、准确。     

双黄补牙周缓释药条体外释放度的测定

目的:建立双黄补牙周缓释药条的质量控制标准,并测定其体外释放度.方法:采用高效液相色谱法(HPLC)作为黄芩苷及盐酸小檗碱的含量测定方法,转篮法测定该药条的体外释放度.结果:双黄补牙周缓释药条中黄芩苷含量为1.63%,盐酸小檗碱含量为0.564%.该缓释药条的释放分为速释和缓释两个阶段.结论:所定的含量测定方法简便、准确可行.双黄补牙周缓释药条具有速释和缓释两个释药系统,符合缓释制剂的设计要求.     

变换波长HPLC法同时测定藿香鼻炎合剂中五种成分的含量

目的建立HPLC波长切换联合梯度洗脱法同时测定藿香鼻炎合剂中的广藿香酮、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素含量的方法。方法采用Kromasil C_(18)(4.6 mm×250 mm,5μm)色谱柱;流动相A:乙腈,流动相B:0.4%磷酸溶液,进行梯度洗脱;流速:1.0 mL/min;柱温:30℃;检测波长分别规定为310 nm(广藿香酮)、280 nm(黄芩苷、汉黄芩苷、黄芩素和汉黄芩素)。结果广藿香酮、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素的线性范围分别为4.300~86.00μg/mL(r=0.999 6)、15.87~317.4μg/mL(r=0.999 8)、6.920~138.4μg/mL(r=0.9999)、6.340~126.8μg/mL(r=0.999 4)、5.250~105.0μg/mL(r=0.999 8),平均加样回收率和RSD均符合中国药典规定。结论本文建立的HPLC波长切换联合梯度洗脱法同时测定广藿香酮、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素5个成分,方法专属性强,重复性好,可作为藿香鼻炎合剂全面可靠的质量控制方法。     

双黄清热颗粒质量标准研究

目的:建立双黄清热颗粒的定性定量方法。方法:采用薄层色谱法对处方中柴胡、金银花、白芍进行定性鉴别;采用HPLC法对处方中黄芩进行含量测定,流动相为甲醇-0.3%磷酸溶液(46:54);检测波长为280nm,流速为1mL.min-1,柱温室温,进样量10μL。结果:双黄清热颗粒定性鉴别特征明显,专属性强;双黄清热颗粒中黄芩苷的含量测定线性范围为0.1192μg～0.5960μg(r=0.9999),平均回收率为99.73%(RSD=0.32%,n=6)。结论:TLC和HPLC方法专属性强、重复性好,可用于控制双黄清热颗粒的质量。     

HPLC法同时测定双黄连片中黄芩苷、绿原酸、连翘苷、连翘酯苷的含量

目的:建立同时测定双黄连片中黄芩苷、绿原酸、连翘苷、连翘酯苷含量的方法。方法:采用高效液相色谱法。色谱柱为Hedera ODS 2柱,流动相为甲醇-0.2%磷酸溶液,采用梯度洗脱,流速为1.0mL.min-1,检测波长为324、280nm,进样量为10μL,柱温为30℃。结果:黄芩苷、绿原酸、连翘苷、连翘酯苷检测浓度分别在28.525～342.3μg.mL-1(r=0.9999)、4.56～54.72μg.mL-1(r=0.9995)、1.55～18.6μg.mL-1(r=0.9994)、1.81～21.72μg.mL-1(r=0.9996)范围内与峰面积积分值线性关系良好;4种成分平均加样回收率分别为98.12%、96.99%、103.16%、100.14%(n=6),均符合含量测定要求。结论:本法简单易行,可用于双黄连片的质量控制。     

高效液相色谱法测定双黄消炎片中黄芩苷和盐酸小檗碱的含量

目的 建立高效液相色谱法同时测定双黄消炎片中黄芩苷和盐酸小檗碱含量的方法。方法采用ODS C18（200mm×4．6mm，5μm）色谱柱，流动相为乙腈0．05mol·L^-1磷酸二氢钾溶液三乙胺（25：75：0．05），流速为1．0mL·min^-1，检测波长为265nm。结果黄芩苷和盐酸小檗碱分别在19．0-380．0μg·mL^-1（r=0．9999）、1．01-20．18μg·mL^-1（r=0．9999）内线性关系良好，平均加样回收率（n=6）分别为100．1％和98．5％。结论该方法简便、准确、重复性好，可同时测定双黄消炎片中黄芩苷和盐酸小檗碱的含量。     

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.