HPLC同时测定万寿菊花中叶黄素及玉米黄素的含量

目的:建立一种同时测定万寿菊花中叶黄素及玉米黄亲含量的HPLC方法。方法:采用Develosil C_(30)色谱桂(250 mm×4．6 mm,5μm),流动相为甲醇-乙腈(49:51),内含0．05％三乙胺,流速1．0 mL·min~(-1),检测波长450 nm。结果:叶黄素和玉米黄素分别在5．0～80．0和2．0～32．0μg·mL~(-1)的浓度内峰面积呈良好的线性关系(r分别为0．9998,0．9997),平均回收率分别为99．25％(RSD=2．1％,n=9)和99．41％(RSD=2．3％,n=9)。结论:本法简便准确、重现性好,可用于万寿菊花中叶黄素及玉米黄素的含量测定。     

测定泰妥拉唑含量的3种方法研究

目的:建立测定泰妥拉唑含量的方法。方法:采用银量法、紫外分光光度法和高效液相色谱法分别对泰妥拉唑进行含量测定。结果:银量法平均回收率为99．9％,RSD为0．13％(n=5),方法精密度为O．09％(n=5); HPLC法在泰妥拉唑浓度为5．020～50．20μg·mL-1的范围内,峰面积与浓度线性关系良好(r=0．999 7),精密度为0．20％(n=6),回收率在99．5％～100．0％;UV法在2．0～12μg·mL-1的范围内线性关系良好(r=0．999 9),精密度为0．81％(n=5),回收率在99．4％～100．3％。结论:3种方法均适用于泰妥拉唑的含量测定,且都有较高的准确度和精密度。银量法结果准确,无需对照品;UV法快速、简便;HPLC法专属性好,可测定主药含量,同时还可进行杂质限度检查。     

高效液相色谱法测定疣克酊中鬼臼毒素的含量

目的:建立疣克酊中鬼臼毒素含量的高效液相色谱测定方法。方法:以Discovery C_(18)(4.6mm×250mm,5μm)为分析柱,以甲醇-水(50:50)为流动相,检测波长285nm,流速为0.8mL·min~(-1)。结果:当鬼臼毒素的浓度在24.8～99.2 mg·L~(-1)范围内时,面积与浓度间呈良好的线性关系(r=0.9999,n=6),方法的平均回收率为98.5％,日内和日间精密度分别为3.8％和4.1％。3批疣克酊剂中鬼臼毒素的百分含量分别为102.00％,101.46％,100.39％。结论:本方法具有准确,简便,灵敏且重现性好的特点,可适用于复方制剂中鬼臼毒素含量的测定。     

高效液相色谱法测定扎莱普隆胶囊的含量

目的:建立测定扎莱普隆胶囊的高效液相色谱法。方法:采用C18色谱柱(150 mm×3．9 mm,5μm),流动相为甲醇-0．02 mol·L-1醋酸铵水溶液(pH 5．00)(60:40),流速0．8 mL·min-1,检测波长232 nm,选用阿普唑仑为内标物。结果:在扎莱普隆浓度为1～100μg·mL-1范围内,扎莱普隆色谱峰面积与内标阿普唑仑色谱峰面积的比值(R)和扎莱普隆浓度(C)呈良好的线性关系,线性方程为:R=2．83×10-2C+4．58×10-2,r=0．999 9,(n=7),扎莱普隆样品与内标物的色谱峰分离完全,两者分离度R>1．5,高、中、低3种浓度的平均加样回收率为98．83％～100．5％,日内精密度(RSD)<0．83％,日间精密度(RSD)<1．6％。结论:该方法灵敏、快速、操作简便、测定结果准确可靠。     

RP-HPLC法测定盐酸拓扑替康及制剂含量和有关物质

目的:建立高效液相色谱法测定盐酸拓扑替康(TPT)及制剂中有关物质和含量。方法:采用十八烷基硅烷键合硅胶为填充剂,0．5％磷酸和0．5％正丁胺(v／v)溶液-甲醇(60:40)为流动相,流速1．0 mL·min-1,检测波长为267 nm。结果:盐酸拓扑替康与有关物质分离良好,线性范围为10-100μg·mL-1(r=0．9999),最低检出量为0．02 ng。方法精密度(RSD)为 0．41％(n=9)。制剂平均回收率为99．3％。结论:方法快速简便,准确,可用于原料及制剂中有关物质和含量的测定。     

高效液相色谱法测定注射用唑来膦酸的含量及有关物质

目的:建立了测定注射用唑来膦酸的含量及有关物质的反相高效液相色谱法。方法:采用C18柱(250 mm×4．6 mm,5μm),以乙腈-四氢呋喃-0．05 mol·L-1磷酸氢二铵(4:1:100,磷酸调节pH值2．55)为流动相用于含量测定,以0．03％氢氧化四丁基铵水溶液(磷酸调节pH值2．55)-乙腈(100:7)为流动相用于有关物质测定。流速1．0 mL·min-1,UV检测波长218 nm。结果:含量测定条件下注射用唑来膦酸在5～125μg·mL-1范围内呈良好的线性关系(r=0．999 9),平均回收率100．3％,RSD=0．50％,有关物质测定条件下,各有关物质与主药的分离良好。结论:本法测定注射用唑来膦酸的含量及有关物质准确可靠。     

HPLC法测定赫酸普鲁卡因葡萄糖注射液中盐酸普鲁卡因和对氨基苯甲酸的含量

目的:用HPLC法同时测定盐酸普鲁卡因葡萄糖注射液中盐酸普鲁卡因和对氨基苯甲酸含量。方法:色谱柱为No- va-Pak C18(150 mm×4．0mm,4μm);流动相为甲醇-10 mmol·L-1NaH2PO4溶液(用磷酸调pH6．48,含2 mmol·L-1三乙胺) (30:70,V／V);流速为0．7 ml·min-1;检测波长为287 nm,柱温30℃。结果:盐酸普鲁卡因浓度在0．1-1．0mg·ml-1范围内线性关系良好(r=0．9989),平均加样回收率98．9％(n=3,RSD=1．4％);对氨基苯甲酸浓度在1-10μg·ml-1范围内线性关系良好(r=0．999 6),平均加样回收率99．2％(n=3,RSD=1．6％)。结论:该方法准确、直观、便于盐酸普鲁卡因葡萄糖注射液质量控制。     

RP-HPLC法测定注射用甲砜霉素甘氨酸酯盐酸盐的含量和有关物质

目的:采用反相高效液相色谱法测定注射用甲砜霉素甘氨酸酯盐酸盐(TGH)含量及有关物质。方法:采用色谱柱:Diamonsil C18柱(250 mm×4．6 mm,5μm);流动相:0．01 mol·L-1三氟乙酸-乙腈(88:12);流速: 1．0 mL·min-1;紫外检测波长:223 nm;进样体积:20μL;柱温:40℃。结果:含量测定的线性范围为40—400μg·mL-1,r=0．999 9(n=5),注射用TGH的加样回收率为98．4％-100．3％;RSD在0．29％-1．08％。结论:本法简便快速、准确,专属性好。     

反相高效液相色谱法测定注射用别嘌醇钠的含量

目的:建立测定反相高效液相色谱法测定注射用别嘌醇钠的含量。方法:采用C_(18)色谱柱(250mm×4．6 mm,5μm);0．125%磷酸二氢钾-甲醇(95:5)为流动相;柱温为30℃;流速为1．0mL·min~(-1);检测波长为230nm。结果:别嘌醇在21．3～149．1μg·mL~(-1)(进样量20μL)之间,样品浓度与峰面积呈良好的线性关系(r= 0．9999),平均回收率为100．7%,RSD为0．84%。结论:本法结果准确,精密度及重现性较好,可准确控制本品质量。     

HPLC法测定盐酸多培沙明含量及有关物质

目的:采用高效液相色谱法测定盐酸多培沙明含量及有关物质。方法:色谱柱为VP-ODS C_(18)柱(150 mm×4．6 mm,5μm),流动相为50 mmol·L~(-1)枸橼酸溶液(含50 mmol·L~(-1)枸橼酸钠)-乙腈(90:10),流速为1 mL·min~(-1),检测波长为280 nm。结果:盐酸多培沙明的线性范围为4～600μg·mL~(-1)(r=0．999 98),平均回收率为99．92％(RSD为0．26％);各杂质峰与主峰达到基线分离。结论:本方法简便、快速,结果准确,重复性好。     

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.