多波长HPLC法同时测定皮肤康洗液中5种有效成分的含量

摘 要 目的：建立多波长切换高效液相色谱法同时测定皮肤康洗液中芍药苷、甘草苷、甘草酸铵、大黄素和蛇床子素5种有效成分的含量。方法: 色谱柱为 Diamonsil C18柱(200 mm×4.6 mm,5 μm);流动相为乙腈 0.1%盐酸水溶液,梯度洗脱;流速为1.5 ml·min^-1;柱温为30℃;检测波长为232 nm(0～6 min,检测芍药苷)、277 nm(6～10 min,检测甘草苷)、254 nm(10 min以后,检测甘草酸铵、大黄素、蛇床子素）。结果: 芍药苷、甘草苷、甘草酸铵、大黄素和蛇床子素的线性范围分别为28.20～282.0 μg·ml^-1（r=0.999 7）、12.150～121.500 μg·ml^-1（r=0.998 8）、13.420～134.200 μg·ml^-1（r=0.999 5）、0.047～0.466 μg·ml^-1（r=0.999 9）、2.380～23.800 μg·ml^-1（r=0.999 9）,平均加样回收率分别为98.49%,99.00%,98.38%,97.36%,97.70%,RSD分别为0.71%,0.62%,0.85%,0.92%,0.78%（n=6）。结论:该方法简便、准确、灵敏度高、重复性好,可用于同时测定皮肤康洗液中上述5个有效成分的含量。     

HPLC法测定黄连上清片中4种成分的含量

摘 要 目的： 提高黄连上清片质量标准,建立同时测定绿原酸、栀子苷、黄芩苷、盐酸小檗碱4种成分含量的方法。方法: 采用高效液相色谱法,色谱柱为DiamonsilTM C₁₈(250 mm×4.6 mm,5 μm),流动相为二元梯度系统,其中溶剂A为乙腈,溶剂B为0.3%磷酸水溶液,流速为1.0 ml·min^-1,检测波长为238 nm,柱温30℃,进样量为10 μl。结果: 绿原酸、栀子苷、黄芩苷、盐酸小檗碱的线性范围分别为8.11～81.10 μg·ml^-1(r=0.999 7)、13.08～130.80 μg·ml^-1(r=0.999 7)、10.76～107.60 μg·ml^-1(r=0.999 8)、7.92～79.20 μg·ml^-1(r=0.999 8)范围内呈良好的线性关系,平均加样回收率分别为99.19%(RSD=0.9%)、98.44%(RSD=1.1%)、99.12%(RSD=1.0%)、99.18%(RSD=1.1%)(n=9)。结论:该方法简便、准确、重复性好,可用于黄连上清片的质量控制。     

HPLC波长切换法同时测定九味双解口服液中5种成分的含量

摘 要 目的：建立HPLC波长切换法同时测定九味双解口服液中绿原酸、咖啡酸、木犀草苷、黄芩苷和大黄素的含量。方法: 采用Shiseido Capcell Pak C₁₈（200 mm×4.6 mm,5 μm）色谱柱,流动相为甲醇（A）-0.1%磷酸溶液（B）（梯度洗脱）,流速为1.0 ml·min^-1,柱温为25℃,检测波长(0~19 min,在327 nm波长下检测绿原酸;19~25 min,在323 nm波长下检测咖啡酸;25~35 min,在350 nm波长下检测木犀草苷;35~55 min,在320 nm波长下检测黄芩苷;55~60 min,在254 nm波长下检测大黄素)。结果: 绿原酸、 咖啡酸、木犀草苷、黄芩苷和大黄素的线性范围分别为0.34～6.8 μg·ml^-1（r=0.999 9）、0.23～4.56 μg·ml^-1（r=0.999 5）、1.32～26.38μg·ml^-1（r=0.999 9）、9.60～192.01μg·ml^-1（r=0.999 9）、1.14～22.80μg·ml^-1（r=0.999 6）;平均加样回收率分别为99.50%（RSD=0.52%）、99.10%（RSD=1.43%）、98.83%（RSD=0.94%）、99.98%（RSD=0.21%）、99.22%（RSD=0.82%）（n=9）。结论:本文建立的含量测定方法,具有操作简便、结果准确、重现性良好的特点,可用于九味双解口服液的质量控制。     

HPLC法同时测定玉真散中天麻素、升麻素苷、5-O-甲基维斯阿米醇苷、欧前胡素、异欧前胡素的含量

摘 要 目的：建立HPLC法同时测定玉真散中天麻素、升麻素苷、5-O-甲基维斯阿米醇苷、欧前胡素、异欧前胡素含量。方法: 色谱柱为Phenomenex Gemini C18柱（250 mm×4.6 mm,5 μm）,柱温为25℃,流速为1.0 ml·min^-1 ,流动相为甲醇 水梯度洗脱,检测波长为230 nm,进样量为5 μl。结果: 天麻素在2.68~214.00μg·ml^-1范围内线性关系良好（r=0.999 9）,平均回收率为100.2％,RSD为0.9％（n=6）;升麻素苷在5.22~418.00 μg·ml^-1范围内线性关系良好（r=0.999 7）,平均回收率为99.9％,RSD为0.9％（n=6）;5-O-甲基维斯阿米醇苷在4.57~365.80 μg·ml^-1范围内线性关系良好（r=0.999 5）,平均回收率为99.7％,RSD为1.0％（n=6）;欧前胡素在5.22~417.20μg·ml^-1范围内线性关系良好（r=0.999 6）,平均回收率为99.0％,RSD为0.9％（n=6）;异欧前胡素在5.29~423.20μg·ml^-1范围内线性关系良好（r=0.999 8）,平均回收率为100.2％,RSD为0.8％（n=6）。结论: 该方法简单、准确,可同时测定5种成分的含量,可用于玉真散的质量控制。     

HPLC法测定枳实消痞丸中芸香柚皮苷、柠檬苦素、和厚朴酚及厚朴酚含量

摘 要 目的： 建立高效液相色谱法同时测定枳实消痞丸中芸香柚皮苷、柠檬苦素、和厚朴酚及厚朴酚含量的分析方法。方法: 色谱柱为岛津Shim-pack VP-ODS C18柱（250 mm×4.6 mm,5 μm）,流动相A为乙腈 甲醇(1∶2),流动相B为水,梯度洗脱,流速为1.0 ml·min^-1,柱温为30℃,进样量为20 μl;芸香柚皮苷检测波长为λ1=283 nm,柠檬苦素检测波长为λ2=210 nm,和厚朴酚、厚朴酚检测波长为λ3=294 nm。结果: 芸香柚皮苷、柠檬苦素、和厚朴酚、厚朴酚分别在5.26～105.20μg·ml^-1（r=0.999 8）、7.65～153.00 μg·ml^-1（r=0.999 4）、6.21～124.20 μg·ml^-1（r=0.999 3）、6.45～129.00 μg·ml^-1（r=0.999 6）范围内线性关系良好,平均加样回收率(n=6)分别为99.00％（RSD=0.77％）、98.17％（RSD=1.19％）、98.78％（RSD=0.86％）、97.90％（RSD=0.99%）。结论:该方法简便、准确、可靠,可用于枳实消痞丸的质量控制。     

HPLC法同时测定蒲药灌肠液中3个有效成分的含量

摘 要 目的： 建立蒲药灌肠液中香蒲新苷、异鼠李素-3-O-新橙皮苷和延胡索乙素的HPLC含量测定方法。方法: 采用ZORBAX SB-C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以乙腈-0.1%磷酸（三乙胺调节pH至6.0）为流动相,梯度洗脱程序,流速:1.0 ml·min^-1,检测波长为254 nm（0～14 min）和281 nm（14～25 min）,柱温:30 ℃。结果: 香蒲新苷、异鼠李素-3-O-新橙皮苷和延胡索乙素的线性范围分别为19.840～198.400 μg·ml^-1（r=0.999 6）、20.520～205.200 μg·ml^-1（r=0.999 8）和10.040～100.400 μg·ml^-1（r=0.999 7）,回收率分别为98.8%、98.6%和98.9%,RSD分别为1.4%、1.6%和1.3%（n=6）。结论: 该方法灵敏度高,专属性强,可用于蒲药灌肠液的质量控制。     

HPLC法同时测定小儿咳喘灵颗粒中6种成分

摘 要 目的：建立利用HPLC法采取波长变换同时测定小儿咳喘灵颗粒中盐酸麻黄碱、（R,S） 告依春、苦杏仁苷、绿原酸、甘草苷、甘草酸含量的方法。方法: 色谱条件：Agilent Eclipse XDB C18（250 mm×4.6 mm,5 μm）,以乙腈 0.1%磷酸为流动相,梯度洗脱,流速为1.0 ml·min^-1 ,测定波长为207 nm（盐酸麻黄碱、苦杏仁苷）、237 nm（甘草酸、甘草苷、绿原酸）、245 nm[（R,S） 告依春）]。结果:盐酸麻黄碱进样浓度在2.423～96.920 μg·m^-1 范围与峰面积线性关系良好,r=0.999 2,平均回收率为100.1%(RSD=0.30%,n=6);（R,S） 告依春进样浓度在1.920～76.798 μg·m^-1 范围与峰面积线性关系良好,r=0.999 9,平均回收率为99.86%(RSD=1.14%,n=6);绿原酸进样浓度在2.396～92.891 μg·m^-1 范围与峰面积线性关系良好,r=0.999 9,平均回收率为98.57%(RSD=0.75%,n=6);苦杏仁苷进样浓度在1.982～79.279 μg·m^-1 范围与峰面积线性关系良好, r=0.999 8,平均回收率为99.67%(RSD=0.59%,n=6);甘草苷进样浓度在2.136～85.440 μg·m^-1 范围与峰面积线性关系良好, r=0.999 9,平均回收率为98.57%(RSD=0.69%,n=6);甘草酸进样浓度在2.432～97.260 μg·m^-1 范围与峰面积线性关系良好,r=0.999 9,平均回收率为98.57%(RSD=0.11%,n=6)。结论:该方法准确、重复性好,可用于小儿咳喘灵颗粒的质量控制。     

HPLC波长切换法测定氨咖黄敏胶囊4个成分的含量

摘 要 目的： 建立HPLC波长切换法同时测定氨咖黄敏胶囊中4个成分的含量。方法: 采用Agilent ZORBAX SB C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以乙腈（A）-甲醇（B）-磷酸二氢铵溶液（取0.1 mol·L^-1磷酸二氢铵溶液1 000 ml ,加磷酸1 ml,混匀）（C）为流动相,梯度洗脱,流速1.0 ml·min^-1,柱温 35℃,变换波长时间为（0～9 min ：225 nm;9～38 min ：450 nm）。结果: 采用HPLC波长切换法测定氨咖黄敏胶囊4个成分的含量,线性范围分别为：对乙酰氨基酚24.680～394.900 μg·ml^-1（r=0.999 9）,马来酸氯苯那敏0.201～3.214 μg·ml^-1（r=0.999 9）,咖啡因1.129～18.070 μg·ml^-1（r=0.999 9）,胆红素0.010～0.165 μg·ml^-1（r=0.999 8）;平均回收率分别为：99.25% (RSD=0.46%), 99.29% (RSD=0.32%),99.49% (RSD=0.48%)及99.75% (RSD=0.55%)（n=6）。结论:该法简单,灵敏,准确,重复性好,可用于氨咖黄敏胶囊的含量测定。     

基于HPLC波长切换法对舒肝益脾液中7种成分的质量控制研究

摘 要 目的：建立HPLC波长切换法同时测定舒肝益脾液中7个成分。 方法: 色谱柱：Luna C18柱（250 mm×4.6 mm,5 μm）;流动相：乙腈 0.05％磷酸溶液,梯度洗脱;流速：0.9 ml·min-1;检测波长：345 nm（滨蒿内酯）、254 nm（毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮和芒柄花素）和210 nm（去氢茯苓酸和茯苓酸）;柱温：30 ℃,进样量：10 μl。结果: 滨蒿内酯、毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮、芒柄花素、去氢茯苓酸、茯苓酸7个成分的线性范围分别为6.09～152.25 μg·ml-1(r=0.999 9)、2.42～60.50 μg·ml-1(r=0.999 8)、1.61～40.25 μg·ml-1(r=0.999 6)、2.95～73.75 μg·ml-1(r=0.999 4)、6.88～172.00 μg·ml-1(r=0.999 9)、2.55～63.75 μg·ml-1(r=0.999 5)、2.09～52.25 μg·ml-1(r=0.999 9);平均加样回收率分别为98.96%（RSD=1.18%）,97.89%（RSD=1.41%）,97.18%（RSD=0.88%）,96.87%（RSD=0.97%）,99.32%（RSD=1.25%）,96.77%（RSD=0.86%）和98.55%（RSD=1.03%）（n=9）。结论: 本文建立的HPLC波长切换法同时测定舒肝益脾液中的7个成分,方法简便,可作为舒肝益脾液全面可靠的质量控制方法。     

HPLC法同时测定大败毒胶囊中绿原酸、咖啡酸和阿魏酸的含量

摘 要 目的: 建立HPLC法同时检测大败毒胶囊中绿原酸、咖啡酸和阿魏酸的测定方法。方法: 采用Agilent C₁₈（250 mm×4.6 mm,5 μm）色谱柱;乙腈-0.4%磷酸溶液（15∶85）为流动相,流速：1.0 ml·min^-1;检测波长：324 nm。柱温:30℃,进样量：10 μl。结果:线性范围：绿原酸5.42～32.43 μg·ml^-1(r=0.999 8),咖啡酸2.63～26.32 μg·ml^-1(r=0.999 4),阿魏酸1.44～14.44 μg·ml^-1(r=0.999 9);平均回收率：绿原酸99.98%,RSD=0.2%(n=6),咖啡酸99.31%,RSD=0.4%(n=6),阿魏酸99.48%,RSD=0.8%(n=6)。结论:该方法操作简便、准确,重复性好,可用于测定大败毒胶囊中绿原酸、咖啡酸和阿魏酸的含量。     

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.