氢化物发生-原子荧光法同时测定六味地黄丸中的砷和汞

目的 :建立六味地黄丸中砷 (AS)和汞 (Hg)同时测定的方法。方法 :采用AFS - 2 30型双道原子荧光光度计 ,以 15 g·L-1硼氢化钠作还原剂 ,1mol·L-1盐酸作载流进行测定。结果 :线性范围砷为 0 .5～ 10 0 μg·L-1,汞为 0 .1～ 6 0 μg·L-1;检出限砷为 0 .0 2 μg·L-1,汞为 0 .0 1g·L-1;加样回收率分别在 99.0 %～ 10 6 .0 % (砷 ) ,89.1%～ 96 .3% (汞 )之间 ,RSD <3.5 % (n =10 )。结论 :方法简便快速 ,结果准确可靠 ,可望作为中成药中重金属元素分析的常规实验方法。     

用HPLC法测定复方对乙酰氨基酚胶囊4组分的含量

目的 :采用HPLC法同时测定复方对乙酰氨基酚胶囊中对乙酰氨基酚、盐酸伪麻黄碱、咖啡因、和马来酸氯苯那敏的含量。方法 :色谱柱为ODSC18,15 0mm× 4 .6mm ;流动相 :甲醇 - 0 .0 5mol/L磷酸二氢钾 三乙胺 (15∶85∶0 .0 2 ) ,用磷酸调pH至 3.4 ,检测波长 2 15nm。结果 :线性范围分别为 :对乙酰氨基酚 5 0～ 35 0 μg·mL-1(r =0 .9997)、盐酸伪麻黄碱 6 .0～ 4 2μg·mL-1(r=0 .9938)、咖啡因 6 .0～ 4 2 μg·mL-1(r =0 .9998)、马来酸氯苯那敏 0 .6～ 4 .2 μg·mL-1(r =0 .9999)。平均回收率分别为 :对乙酰氨基酚 10 2 .3%、盐酸伪麻黄碱 10 0 .9%、咖啡因 10 1.8%、马来酸氯苯那敏 10 1.5 %。结论 :本法分离度好 ,快速 ,简便 ,可同时测定该胶囊中的四组分。     

顶空气相色谱法测定几丁糖酯中溶剂残留

目的 :建立顶空气相色谱法分析几丁糖酯中溶剂残留。方法 :采用水溶液顶空和固体顶空 2种气相色谱法 ,用AC -2 0石英毛细管色谱柱 ,以正丙醇为内标进行定量。结果 :水溶液顶空气相色谱法乙醇的线性范围为 8～ 192 μg·mL-1,丙酮的线性范围为 2～ 6 4μg·mL-1;方法的回收率为乙醇 10 3 3% ,丙酮 95 71% ,RSD均为 4 2 % ;最低检测限溶液中乙醇为 4μg·mL-1,丙酮为 1μg·mL-1。固体顶空气相色谱法乙醇的线性范围为 0 16～ 2 4μg·mL-1,丙酮的线性范围为 0 16～ 1 6 μg·mL-1;方法的回收率为乙醇 96 32 % ,丙酮 10 2 1% ,RSD分别为 3 5 %和 2 6 % ;最低检测限乙醇为 0 12 μg·g-1,丙酮为 0 0 6 μg·g-1。结论 :此 2种方法简单 ,准确 ,灵敏度高 ,经显著性检验二者无显著性差异。     

RP—HPLC法同时测定来氟米特及A771726

目的 :建立反相高效液相色谱同时测定来氟米特及A77172 6的方法。方法 :采用HypersilODSC18柱 ,乙腈-醋酸盐缓冲液为流动相 ,检测波长分别为 2 6 0nm及 2 90nm ,流速 1 40mL·min-1,进样量 2 0 μL ,肉桂酸为内标。结果 :能同时测定来氟米特及A77172 6 ,来氟米特线性范围 0 79～ 31 6 0 μg·mL-1(r =0 9999) ,平均回收率为 10 0 3% (RSD =0 76 % ) ;A77172 6线性范围 0 35～ 14 0 0 μg·mL-1(r =0 9996 ) ,平均回收率为 99 6 9%(RSD =0 95 % )。结论 :本法简便、快速、准确     

反相离子对高效液相色谱法测定泰必治注射液A中4种组分的含量

目的 :采用反相离子对高效液相色谱法测定泰必治注射液A中盐酸利多卡因、地塞米松、卡巴芬乙酸 (钠盐 )与保泰松钠 4种组分的含量。方法 :采用YWG -C1 8(10 μm ,4 5mm× 15 0mm)色谱柱 ,以乙腈 -水 (4 5∶5 5 ,含 2 5mmol·L- 1十六烷基三甲基溴化铵 )为流动相 ,流速 1 5mL·min- 1 ,柱温 40℃ ,检测波长 2 30nm。结果 :本法可同时测定 4种组分的含量。盐酸利多卡因在 13～ 6 4μg·mL- 1 、地塞米松在 4 5～ 38μg·mL- 1 、卡巴芬乙酸 (钠盐 )在 2 6 9～ 16 14μg·mL- 1 、保泰松钠在 40 2～ 2 0 77μg·mL- 1 范围内 ,峰面积与其浓度呈良好的线性关系 ;平均回收率 (n =5 )依次为 99 9% (RSD =1 2 % ) ,10 1 0 % (RSD =0 4% ) ,10 0 5 % (RSD =0 2 % ) ,10 0 6 % (RSD =0 8% )。结论 :方法简便、快速、准确 ,可作为样品的检测方法。     

HPLC法测定咖普苯片中咖啡因、盐酸普萘洛尔、苯妥英钠3组分的含量

目的 :建立同时测定咖普苯片中咖啡因、盐酸普萘洛尔、苯妥英钠 3组分含量的高效液相色谱法。方法 :采用In ertsil-ODS柱 ,流动相为甲醇 -水 - 0 2mol·mL-1磷酸二氢钾溶液 (5 0∶43∶2 ) ,流速 1 0mL·min-1,检测波长 2 30nm ,外标法计算。结果 :线性范围分别是 :咖啡因 2 0～ 16 0 μg·mL-1,r =0 9998;盐酸普萘洛尔 3～ 2 4μg·mL-1,r =0 9995 ;苯妥英钠 35～ 2 80 μg·mL-1,r =0 9999。回收率 :咖啡因 10 0 3 % ;盐酸普萘洛尔 10 0 7% ;苯妥英钠98 6 %。结论 :本方法分离效果好 ,辅料无干扰 ,快速、简便 ,适用于该制剂 3组分的同时测定     

高效液相色谱法测定复方替硝唑搽剂中替硝唑和水杨酸的含量

目的 :建立测定复方替硝唑搽剂中替硝唑和水杨酸含量的高效液相色谱法。方法 :采用反相ODS色谱柱 ,甲醇 - 0 0 2mol·L-1KH2 PO4 溶液 (5 0∶5 0 )为流动相 ,检测波长为 315nm。结果 :替硝唑和水杨酸的线性范围分别在5 0～ 35 0 μg·mL-1(r=0 9997) ,40 0～ 16 0 0 μg·mL-1(r =0 9997) ;加样回收率分别为 10 0 6 % (RSD =0 6 9% )及 10 0 6 % (RSD =0 79% ) ;日内RSD为 0 16 %～ 1 2 %和 0 6 1%～ 1 2 % ,n =12 ,日间RSD为 0 2 4%～ 1 7%和0 2 %～ 1 1% ,n =4。结论 :HPLC法可用于复方替硝唑搽剂的含量测定 ,方法准确、灵敏 ,专属性强     

离子对—反相高效液相色谱法测定苄达赖氨酸及其滴眼液的含量

目的 :研究离子对 -反相高效液相色谱法测定苄达赖氨酸及其滴眼液的含量 ,增加质量控制手段。方法 :采用庚烷磺酸钠作反离子 ,AlltimaC18色谱柱 ,以甲醇 -水 -冰醋酸 (6 4∶36∶0 5 ) ,内含 0 5mmol·L-1庚烷磺酸钠为流动相 ,紫外检测波长 30 7nm ,流速 1 0mL·min-1,柱温 30℃。结果 :在 30～ 2 0 0 μg·mL-1浓度范围内呈良好线性 ,最低检测浓度为 0 5 μg·mL-1,日内、日间精密度 (RSD)分别为 0 6 % (n =4)和 0 9% (n =3) ,平均加样回收率为 10 1 7% ,RSD =0 8% (n =5 )。结论 :该方法分析速度快 ,操作简便 ,准确 ,灵敏度高 ,专属性好 ,可作为该药制剂的含量测定方法     

HPLC同时测定血清中苯妥英、苯巴比妥和卡马西平的浓度

目的 :建立同时测定微量血清中苯妥英、苯巴比妥和卡马西平浓度的方法。方法 :采用HPLC法 ,以巴比妥为内标同时测定。KromasilC18不锈钢色谱柱 ,流动相为甲醇 水 (5 7∶43) ,流速 0 .8ml·min 1,检测波长 2 5 4nm。结果 :检测浓度范围苯妥英为 4.0～ 5 0 .0 μg·ml 1(r=0 .9995 ) ,苯巴比妥 5 .0～ 6 0 .0 μg·ml 1(r =0 .9996 ) ,卡马西平为2 .5～ 2 0 .0 μg·ml 1(r =0 .9992 )。最低检测限分别为 1.0 μg·ml 1、2 .0 μg·ml 1和 0 .5 μg·ml 1;平均回收率分别为99.2 2 %、99.6 8%和 98.6 2 % ;日内和日间RSD均低于 5 % (n =5 )。结论 :该法准确、灵敏度高 ,重复性好 ,可作为 3种血药浓度监测的常规方法     

高效液相色谱法测定克林沙星血药浓度

目的 :建立用高效液相色谱法测定血浆中克林沙星浓度的方法。方法 :血浆样品在酸性条件下 ,以Oasis小柱提取环丙沙星为内标 ,采用LichrosorbC18(5 μm)柱 ,流动相为乙腈 - 0 0 5mol·L-1柠檬酸三乙胺溶液 (pH 2 5 ) (2 0∶80 ) ,流速为 1 0mL·min-1,检测波长 30 0nm ,克林沙星和内标的保留时间分别为 7 1min和 4 5min。结果 :线性范围在 0 0 3～10 μg·mL-1(r=0 9998) ,最低检测浓度为 0 0 2 μg·mL-1,RSD <7%。用本法测定了 6只大鼠灌胃剂量 5 0mg·kg-1克林沙星后血浆中克林沙星的浓度经时变化过程。结论 :本方法可用于克林沙星的血药浓度测定及药代动力学研究。     

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.