RP-HPLC测定复方麻黄碱滴鼻液中盐酸麻黄碱、盐酸林可霉素和地塞米松磷酸钠含量的方法学研究

目的 建立反相高效液相色谱法测定复方麻黄碱滴鼻液中盐酸麻黄碱、盐酸林可霉素和地塞米松磷酸钠含量的方法.方法采用Dikma C18(150 mm x4.6 mm,5μm)色谱柱,甲醇-0.05mol·L-1硼砂缓冲液(用磷酸调节pH值至6.0)(4753)为流动相,检测波长为241nm.结果盐酸麻黄碱、盐酸林可霉素、羟苯乙酯(尼泊金乙酯)和地塞米松磷酸钠的分离度完全达到要求.盐酸麻黄碱浓度在2.55～30.63 mg·mL-1内线性关系良好(r=0.999 9);盐酸林可霉素在2.58～30.98 mg·mL-1内线性关系良好(r=0.999 6);地塞米松磷酸钠在49.53～594.30 μg·mL-1内线性关系良好(r=1.000 0);平均回收率分别为99.75%(RSD为0.77%)、102.11%(RSD为0.94%)、99.69%(RSD为0.72%).结论 本方法准确、专属、简便、快速,能有效地控制产品的质量.     

HPLC法测定盐酸美他环素片的含量

目的:建立外标法测定盐酸美他环素片含量的高效液相色谱方法.方法:采用PurospherStar C18色谱柱(250 mm×4.6 mm,5 μm);流动相:甲醇-水(50:50)混合后用磷酸调节pH至3.0±0.02;检测波长:280 nm;进样体积:20 μL,流量:0.7 mL·min-1;温度35℃.结果:美他环素在20.02～200.2 μg·mL-1浓度范围内线性关系良好(r=0.999 9);平均回收率为98.6%,RSD为0.6%.结论:本测定方法简便快速,灵敏度高,准确度好,可用于盐酸美他环素片的含量测定.     

1%盐酸林可霉素乳膏的制备及质量控制

目的:制备盐酸林可霉素乳膏并建立其质量控制方法.方法:以水包油基质制备乳膏;采用高效液相色谱法测定盐酸林可霉素的含量;色谱柱:Hypersil C18柱(250 mm×4.6 mm,5 μm);流动相:磷酸缓冲液(pH=6.8)-甲醇(40:60);流速0.8ml·min-1;检测波长:214 nm;柱温:30℃.结果:制剂各项检查均符合<中国药典>2005年版相关规定;盐酸林可霉素的线性范围为0.240 2～0.560 6 mg·ml-1(r=0.999 8),平均回收率为99.7%.结论:本制剂制备工艺简便,控制方法快速、准确.     

高效液相色谱-紫外检测法测定健康人血浆和尿中法罗培南浓度

目的建立高效液相色谱-紫外检测方法,检测健康人血浆和尿中法罗培南(β内酰胺类抗生素)浓度。方法色谱柱为YMC—Pack ODS—A(5 μm,250 mm×4．6 mm)流动相用0．02 mol·L-1磷酸二氢钠(pH 2．4)-乙腈溶液=(75:25),流量为0．9 mL·min-1,UV波长为318 nm,替硝唑为内标。结果血浆:法罗培南在0．05～10．0 μg·mL-1内线性良好,标准曲线方程为γ=2．46x-9×10-4(γ=0．9995,n=5),方法回收率在87．37％- 94．02％,日内RSD≤7．13％,日间RSD≤17．84％。尿:法罗培南在0．25～ 200．0 μg·mL-1内线性良好,标准曲线方程为γ=2．87×10-2x 1．45×10-2 (γ=0．9996,n=5),方法回收率在99．44％～103．61％,日内RSD≤8．73％, 日间RSD≤14．11％。结论本方法样品处理简单、快速、准确,灵敏度好,适用于临床药代动力学及生物等效性研究。     

HPLC法测定硫酸头孢匹罗的含量及有关物质

目的:建立硫酸头孢匹罗含量及其有关物质的HPLC检测方法.方法:采用Lichrospher-C18色谱柱(250 mm×4.6 mm,5 μm);流动相为 0.03 mol·L-1磷酸二氢铵缓冲液(pH3.3)-乙腈(9:1),流量 1.0 mL·min-1,检测波长 270 nm.结果:硫酸头孢匹罗在149.1～347. 9 μg·mL-1浓度范围内线性关系良好(r=0.9999),与中间体1、中间体2及副产物完全分离,中间体1和中间体2的最低检测浓度分别为 27.2 ng·mL-1、25.8 ng·mL-1.结论:本测定法简便快速,灵敏度高,准确可靠,可同时测定硫酸头孢匹罗的含量及有关物质.     

HPLC法测定复合维生素B片中维生素B1、B2、B6的含量

目的 建立高效液相色谱法测定复合维生素B片中维生素B1、维生素B2、维生素B6的含量.方法 色谱柱:Wondasil C18色谱柱,流动相为醋酸-醋酸钠缓冲液(pH 4.5)-甲醇(65∶35),流速为1.0 mL·min-1,检测波长为270 nm.结果 维生素B1、维生素B2、维生素B6浓度分别在0.6 μg·mL-1～0.75 mg·mL-1、0.3 μg·mL-1～0.62 mg·mL-1、80～415 μg·mL1范围内与峰面积线性关系良好.结论 该方法简便、快速、准确可靠,可用于复合维生素B片中维生素B1、维生素B2、维生素B6的含量测定.     

IC法测定托吡酯胶囊中氨基磺酸盐和硫酸盐

目的 建立检测托吡酯胶囊中氨基磺酸盐和硫酸盐的离子色谱方法.方法 采用Dionex IonPac AS14A分析柱(250 mm×4 mm),前接IonPac AG14A保护柱(50 mm×4 mm),外接ASRS300抑制器,以碳酸盐缓冲液(508.8 mg无水碳酸钠与84.0 mg碳酸氢钠,溶于1 000 mL水中)为淋洗液,流速为1.0 mL·min-1,进样量为25 μL,检测器温度为30 ℃.结果 空白溶液不干扰本品中氨基磺酸盐和硫酸盐的检测,氨基磺酸盐(以NH2SO3-计)的回归方程为A=0.130 5C-0.001 9(n=7),在0.077 8~9.340 8 μg·mL-1浓度范围内线性关系良好(r=0.999 6),平均回收率为100.16%,RSD为2.08%(n=9),检测限为0.03 μg·mL-1,定量限为0.08 μg·mL-1;硫酸钠(以SO42-计)的回归方程为A=0.306 9C+0.009 6(n=7),在0.112 7~13.524 0 μg·mL-1浓度范围内线性关系良好(r=1.000 0),平均回收率为101.44%,RSD为1.31%(n=9),检测限为0.10 μg·mL-1,定量限为0.23 μg·mL-1.结论 该方法简便、快速、准确、专属性强、灵敏度高、重现性好,可用于托吡酯胶囊中氨基磺酸盐和硫酸盐的测定.     

高效液相色谱法测定盐酸多巴酚丁胺注射液中依地酸二钠的含量

目的 建立盐酸多巴酚丁胺注射液中依地酸二钠的含量测定方法.方法 色谱柱为Hibar C18(250mm×4.6mm,5μm),流动相为0.3％四丁基氢氧化铵溶液(pH=4.0)-水-乙腈(18∶45∶37),检测波长为254nm,流速为1.0mL·min-1,进样量为20μL.样品经稀释后加醋酸铜溶液7mL,直接进样分析.结果 依地酸二钠浓度在6.960-116.1μg·mL-1线性关系良好(r=0.9999);检出限为0.46 μg· mL-1;样品平均回收率(n=9)为101.3％.结论 本方法简便、准确、灵敏度高、重复性好,可用于盐酸多巴酚丁胺注射液中依地酸二钠的含量测定.     

反相高效液相色谱法测定盐酸青藤碱纳米脂质体药物含量及包封率

目的建立盐酸青藤碱纳米脂质体药物含量及包封率的测定方法.方法采用反相高效液相色谱法,以十八烷基硅烷键合硅胶为固定相,以甲醇-0.01 mol·L-1NaH2PO4(38∶62)为流动相;柱温为30 ℃;流速为1 mL·min-1;检测波长为262 nm.采用透析法分离盐酸青藤碱游离药物.结果在所选定的色谱条件下辅料及溶剂对盐酸青藤碱的测定无干扰,盐酸青藤碱在5～80 μg·mL-1线性关系良好(r=0.999 9);回收率为99.6%～101.1%,日内和日间RSD均＜2%(n=5).结论该方法准确可靠、简单快速,可用于盐酸青藤碱纳米脂质体含量及包封率的测定.     

HPLC-RID法测定氨糖美辛肠溶片中盐酸氨基葡萄糖含量

建立高效液相色谱-示差折光检测器法测定氨糖美辛肠溶片中盐酸氨基葡萄糖含量。方法：使用Waters XBridge Amide (4.6 mm×250 mm,3.5 μm) 色谱柱,流动相：80%乙腈溶液(1 000 mL中含1 mL氨水),流速：1.2 mL·min-1;柱温： 40 ℃;进样量：20 μL,示差折光检测器（RID）检测。结果：盐酸氨基葡萄糖检测限为0.03 mg·mL-1,定量限为0.125 mg·mL-1,其在0.72~7.56 mg·mL-1质量浓度范围内呈良好的线性关系。平均回收率为99.36% （RSD=0.85%,n=9）。测定氨糖美辛肠溶片7批,盐酸氨基葡萄糖的含量在93%~107%范围内。结论：所建方法检测快速准确、专属性强、耐用性较好,可用于盐酸氨基葡萄糖含量的测定,为有效控制氨糖美辛肠溶片的质量提供参考。     

Nachweis einiger Heilmittel in der Kniegelenksynovialflüssigkeit

Zusammenfassung Mittels Gaschromatographie und Dünschichtchromatographie wiesen die Autoren 11 Substanzen nach, welche durch Injektion oder nach Verabreichung per os in die Kniegelenksynovialflüssigkeit eindrangen. In ihrer Aufstellung konnten sie eine direkte Beziehung zwischen Struktur sowie chemischphysikalischen Eigenschaften der Substanz und ihrer Fähigkeit, aus dem Blut in die Kniegelenksynovialflüssigkeit einzudringen, nicht nachweisen, außer der Tatsache, daß Substanzen mit starker Affinität zu Eiweißstoffen erst in höheren Dosen nachweisbar waren.     

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.     

Emerging drugs for epilepsy

Epilepsy affects ≤ 1% of the world's population. Antiepileptic drugs (AEDs) are the mainstay of treatment, although more than a third of patients are not rendered seizure free with existing medications. Uncontrolled epilepsy is associated with increased mortality and physical injuries, and a range of psychosocial morbidities, posing a substantial economic burden on individuals and society. Limitations of the present AEDs include suboptimal efficacy and their association with a host of adverse reactions. Continued efforts are being made in drug development to overcome these shortcomings employing a range of strategies, including modification of the structure of existing drugs, targeting novel molecular substrates and non-mechanism-based drug screening of compounds in traditional and newer animal models. This article reviews the need for new treatments and discusses some of the emerging compounds that have entered clinical development. The ultimate goal is to develop novel agents that can prevent the occurrence of seizures and the progression of epilepsy in at risk individuals.     

盐酸达泊西汀中甲磺酸甲酯、甲磺酸乙酯及甲磺酸异丙酯的顶空毛细管GC-ECD法测定

建立了衍生化顶空毛细管气相色谱-电子捕获检测器(ECD)法测定盐酸达泊西汀中的甲磺酸甲酯(MMS)、甲磺酸乙酯(EMS)和甲磺酸异丙酯(IMS).应用碘化钠衍生技术,使用PW-5毛细管柱,载气为氮气,ECD检测,程序升温.MMS、EMS和IMS分别在0.03～0.30、0.05～0.50和0.05～0.50 μg/ml浓度范围内线性关系良好,平均回收率分别为63.5％、100.3％和96.2％,最低检测限分别为0.30、0.50和0.50 ng/ml.     

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.