高效液相色谱法测定大鼠血中头孢他啶浓度的实验

本文报告采用高效液相色谱法（ＨＰＬＣ）测定大鼠血中的头孢他啶浓度。样品在酸性条件下转入水相，样品中杂质在中性条件下转入混合溶媒。色谱柱为ＹＷＧ－Ｃ１８柱，内标物选用氢氯噻嗪。流动相为０．１ｍｏｌ·Ｌ－１醋酸铵缓冲液（ｐＨ４．５９）与甲醇按８８∶１２配成的混合液。最低检出浓度为０．２μｇ·ｍｌ－１，日内相对标准偏差在３．３％以内，日间相对标准偏差在４％～１２％之间。本法操作简便、快速、专一性强、重现性好。     

用HPLC法同时测定皮肤渗透液中18-甲墓炔诺酮和雌二醇的含量

用ＨＰＬＣ法同时测定皮肤渗透液中１８－甲基炔诺酮和雌二醇的含量。色谱柱：Ｓｈｉｍ－ＰａｃｋＣＬＣ－ＯＤＳ，检测波长：２８０ｎｍ（０—７．２０ｍｉｎ），２４２ｎｍ（７．２１—８．９０ｍｉｎ），流动相：甲醇－水（７５：２５）．线性范围均为０．２～４．０μｇ／ｍｌ（ｒＬＮＧ＝０．９９９９，ｒＥ２＝０．９９９８）；最低检测量ＬＮＧ为１ｎｇ，Ｅ２为５ｎｇ，ＬＮＧ与Ｅ２在等浓度条件下平均回收率分别为ＬＮＧ１００．６４±０．７５％，Ｅ２　９９．９９±０．８４％，日内ＲＳＤ分别为ＬＮＧ０．４４％，Ｅ２１．０６％，日间ＲＳＤ分别为ＬＮＧ０．７８％，Ｅ２　１．３０％。该方法简便、快速，结果准确。     

复方β—胡萝卜素胶囊的RP—HPLC测定

以ＹＷＧ－Ｃ１８为色谱柱，无水乙醇－水－８５％磷酸（９６∶４∶０．０２）为流动相，检测波长为２８０ｎｍ，采用ＲＰ－ＨＰＬＣ法同时测定复方β－胡萝卜素胶囊中两组分的含量。维生素Ｅ和β－胡萝卜素平均回收率分别为１００．５％和９９．４％，ＲＳＤ分别为０．３％和０．８％。     

反相HPIC法测定血清布洛芬含量

本文以消炎痛为内标，用反相ＨＰＩＣ测定血清中的布洛芬。色谱柱为ＹＷＧＣ（１８）（１０μｍ）２００ｍｍ×５ｍｍ。流动相为甲醇－２０ｍｍｏｌ／Ｌ。磷酸二氢钾缓冲液（７０：３０，ｐＨ３．８）。流速为１ｍｌ／ｍｉｎ。检测波长为２２５ｎｍ。色谱柱柱温为５０℃。布洛芬和内标的保留时间分别为７．２和５．２ｍｉｎ。布洛芬的检测限为２ｎｇ（Ｓ／Ｎ≥４：１）。血清样品的预处理采用１：１的乙腈沉淀蛋白后直接进样。血清布洛芬浓度在０．５～６４μｇ／ｍｌ范围呈线性关系（ｒ＝０．９９９６）。天内天间精密度分别为１．６％～３．９％和２．１％～５．０％。     

地匹福林的反相离子对色谱法分析研究

本文建立了用反相离子对色谱法测定地匹福林及其制剂的方法。并对色谱条件进行了优化，选用国产色谱柱（ＹＷＧ－Ｃ１８，１０μ），流动相为甲醇－０．３ｍｏｌ／Ｌ ＮａＣｌＯ４／０．０１ｍｏｌ／Ｌ ＨＣｌＯ４（６８：３２），检测波长为２５４ｎｍ，萘为内标。方法的线性范围为４～７０μｇ，相关系数为０．９９９８，实验测得地匹福林原料药和其制剂的平均回收率分别为９９．９％和９９．４％，相对标准偏差分别为１．２％和     

HPLC法测定心脑脉舒口服液中阿魏酸含量

本文建立了心脑脉舒口服液中阿魏酸含量测定方法。色谱柱：ＹＷＧ－Ｃ１８，４．０×１５０ｍｍ；流动相：甲醇－水－冰乙酸（３３：６６：１）；流速：１．０ｍ１／ｍｉｎ；ＵＶ检测波长：３２０ｍｍ。结果表明，方法快速、准确、灵敏、重现性好。阿魏酸浓度在０．２～１．０μｇ／μ１范围内线性关系良好（γ＝０．９９９８），加样回收率为９６．７４％，ＲＳＤ＝２．７％，实际测定１０批样品结果满意。     

气相色谱法测定脉通中亚油酸含量

以氢氧化钾－甲醇溶液和三氟化硼－甲醇溶液为试剂，将亚油酸转变为亚油酸甲酯，以正辛烷为溶媒，取上清液，在丁二醇二乙二醇聚酯（ＤＥＧＳ）柱上，采用外标法进行气相色谱分析，方法简便可靠，重现性好，相关系数ｒ为０．９９９８，回收率均值为１０１．０％，变异系数为１．２５％。     

HPLC法测定吗氯贝胺片的含量

建立了测定片剂中吗氯贝胺的ＨＰＬＣ方法，色谱条件为ＷａｔｅｒｓＣ１８色谱柱，乙腈－０．０５ｍｏｌ／Ｌ醋酸铵溶液－冰醋酸（２５：７５：１．５）为流动相，２５４ｎｍ检测波长，咖啡因为内标，该法简便，灵敏，准确，吗氯贝胺在１９．８～１９８．０ｍｇ／Ｌ浓度内线性关系良好（ｒ＝０．９９９９），平均回收率为１００．０％，（ＲＳＤ＝０．１７％，ｎ＝５）。     

高效液相色谱法测定人血清中5-氟尿嘧啶的浓度

目的：测定 ５－氟尿嘧啶在人血清中的浓度。方法：三氯乙酸沉淀血清中蛋白质,高效液相色谱法测定含量。色谱柱为 ＳｈｉｍｐａｃｋＣＬＣ Ｃ１８柱,加 ＹＷＧ预柱;流动相为 ０．２５％磷酸二氢钾－乙腈（９８：２）,ｐＨ７．０;流速为 １ｍｌ／ｍｉｎ;紫外检测波长 ２６５ｎｍ。分别在低浓度范围（０．１９５～６．２５０μｇ／ｍｌ）和高浓度范围（６．２５０～２００．００μｇ／ｍｌ）制作标准曲线以用于定量。结果：５－氟尿嘧啶在 ０．１９５～２００μｇ／ｍｌ浓度范围呈良好的线性关系,０．８、４、２０和１００μｇ／ｍｌ４个浓度点的日内平均回收率和ＲＳＤ分别为１０４．８８％、１．９５％,１０４．５８％、１．３８％,１０１．４０％、０．３９％,９９．１４％、０．３７％;日间平均回收率和ＲＳＤ分别为１０５．１２％、２．０２％,１０６．３０％、０．７８％,１００．６０％、０．６５％,９９．３８％、０ ９２％。结论：本文建立的方法快速、准确,适合于５－氟尿嘧啶的药代动力学研究和常规血药浓度监测。     

用HPLC测定大鼠体液和组织中的环氧司坦

本文建立了高效液相色谱法（ＨＰＬＣ）测定大鼠血浆、胆汁、尿、粪和肝组织中的环氧司坦浓度。采用ＹＷＧ－Ｃ（１８）Ｈ（３７）柱，甲醇－０．５％四甲基乙二胺缓冲溶液（８０：２０，Ｖ／Ｖ）为流动相，内标为甲基睾丸素，ＵＶ检测波长２５４ｎｍ。血浆样品用环己烷－异丙醇（９７：３，Ｖ／Ｖ）提取，色谱峰分离完全，方法线性良好，ｒ＝０．９９９８，提取回收率为７７．０±５．８％，方法回收率８８．０±５．６％，日内ＲＳＤ为０．６５％～０．７８％，日间ＲＳＤ为２．０２％～３．７７％；胆汁、尿、粪、肝组织的ｒ值分别为０．９９９７、０．９９９８、０．９９９６、０．９９９８，其平均回收率为６８．５５±５．７％、８８．１７±４．２７％、９２．１７±１．０９％、８１．５５±１．４６％。用本法测定大鼠灌胃（ｉｇ）环氧司坦５０ｍｇ／ｋｇ后的药代动力学，并报道了有关参数。     

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.