HPLC法同时测定三七中7种皂苷含量

目的：建立HPLC法同时测定三七中7种皂苷含量的方法。方法：Hypersil BDS C18色谱柱（250mm×4．6mm，5μm）；流动相：乙腈（A）-水（B）二元梯度洗脱；流速：1．0ml·min^-1；检测波长203nm；柱温：室温。结果：三七皂苷R1，人参皂苷Rb1，Rb2，Rc，Rd，Rg1，Re的线性范围分别为5．6～140μg·ml^-1（r=0．9992）5．8～144μg·ml^-1（r=0．9991）、5．9-148μg·ml^-1（r=0．9997）、6．1～152μg·ml^-1（r=0．9992）、5．8～144μg·ml^-1（r=0．9992）、5．8～146μg·ml^-1（r=0．9990）、5．8～144μg·ml^-1（，=0．9994）；回收率98．5％～100．1％。结论：HPLC法可同时并且简单快速分离三七中7种皂苷。     

高效液相色谱法测定beagle犬血浆中神衰果素的浓度

目的：建立高效液相色谱法（HPLC）测定beagle犬血浆中神衰果素的含量的方法。方法：色谱柱采用Diamon-sil ODS C18柱（4．6mm×150mm，5μm），以乙腈-甲醇-0．02mol·L^-1磷酸二氢钠缓冲液（1：9：90）（磷酸二氢钠缓冲液用磷酸调pH3．0）为流动相，原儿茶醛为内标；流速为1．0mL·min^-1；柱温为30℃；检测波长为270nm。结果：HPLC法测定beagle犬血浆中神衰果素的线性范围为21．3-4260μg·L^-1，r=0．9995.低（42．6μg·L^-1）、中（426μg·L^-1）、高（2130μg·L^-1）3个质量浓度的方法回收率分别为（96．7±13．5）％，（95．6±7．6）％，（99．9±1．4）％，日内、日间RSD均小于15％；分析方法的最低定量限为21．3μg·L^-1。结论：本方法适用于神衰果素血药浓度测定和药动学研究。     

反相高效液相色谱法测定口腔溃疡涂剂中甲硝唑和盐酸丁卡因的含量

目的：建立以反相高效液相色谱法测定口腔溃疡涂剂中甲硝唑和盐酸丁卡因含量的方法。方法：色谱柱为Thermo ODS hypersilC18（50mm×4．6mm，5μm）；流动相为甲醇-水-乙腈-三乙胺（35：50：15：0．7）（用冰醋酸调pH=6．8）；流速1．0ml·min^-1；检测波长为310nm；柱温20℃。结果：甲硝唑和盐酸丁卡因分别在20．2～161．6μg·ml^-1（r=0．9994）和6．68～53．44μg·ml^-1（r=0．9993）范围内线性关系良好，平均回收率分别为99．89％（RSD0．62％）和99．84％（RSD0．67％）。结论：本法简便、快速、重复性好，可用于口腔溃疡涂剂的质量控制。     

HPLC法测定苦参药材中苦参碱的含量

目的：建立测定苦参药材中苦参碱含量的高效液相色谱法。方法：采用Alltech Alltima C18（250mm×4．6mm，5μm）色谱柱，柱温25℃；流动相为0．02mol·L^-1三乙胺（醋酸调节pH9．5）-乙腈（60：40），流速1．0mL·min^-1；检测波长为220nm。结果：线性范围为0．01～2．0mg·mL^-1；稳定性试验RSD为0．57％（n=5）；平均回收率为99．42％（n=6）；重复性试验RSD为1．78％（n=6）。结论：本方法快速简便、准确，重复性好。     

HPLC法测定盐酸左旋咪唑糖浆的含量

目的：采用高效液相色谱法测定盐酸左旋咪唑糖浆的含量。方法：采用Agilent TC—C18色谱柱（4．6mm×150mm，5μm）；以0．05mol·L^-1磷酸二氢钾溶液（二乙胺调节pH7．0）-乙腈（60：40）为流动相；流速1．0mL·min^-1；检测波长为215nm；柱温：室温。结果：盐酸左旋咪唑线性范围为5．14～25．70μg·mL^-1（r=0．9998），平均回收率（n=6）为98．3％，RSD为0．56％。结论：本方法简便、准确、重现性好，可用于测定盐酸左旋咪唑糖浆的含量。     

HPLC法同时测定炎菌清搽剂中水杨酸、醋酸曲安奈德和利福平的含量

目的：建立高效液相色谱法同时测定炎菌清搽剂中水杨酸、醋酸曲安奈德、利福平的含量。方法：采用高效液相色谱法，色谱柱为Hypersil C18（4．6mm×250mm，5μm），流动相为甲醇-乙腈-0．075mol·L-1磷酸二氢钾溶液-1．0mol·L-1枸橼酸溶液（30：30：26：4），流速0．8mL·min-1，检测波长254nm，柱温30℃。结果：水杨酸、醋酸曲安奈德、利福平的线性范围分别是：202．24～2022．4μg·mL-1（r=0．9991），5．2—52μg·mL-1（r=0．9994），20．23～202．3μg·mL-1（r=0．9996）；日内精密度RSD（n=5）分别是1．4％，1.2％，0．89％；平均回收率（n=9）分别为100．6％，97．8％，100．5％。结论：本方法快捷方便，结果可靠，可作为炎菌清搽剂的质量控制标准。     

高效液相色谱法测定苯妥英钠凝胶剂的含量

目的：建立了高效液相色谱法测定苯妥英钠凝胶剂的含量。方法：采用Hypersil ODS-2C18色谱柱（250mm×4．6mm，5μm）；流动相为0．05mol·L-1磷酸二氢钾（pH3．5）-甲醇（53：47）；流速1．0mL·min；检测波长220nm；柱温：35℃。结果：苯妥英钠在1—20μg·mL-1浓度范围内线性关系良好（r=0．9998）；平均回收率为100．1％（n=9）。结论：本方法简单，灵敏，重现性好，可用于苯妥英钠凝胶剂的含量测定。     

HPLC测定维药祖卡木胶囊中大黄素、大黄酚的含量

目的：采用高效液相色谱法测定祖卡木胶囊中大黄素和大黄酚的含量。方法：采用Waters Symmetry C18（150mm×4．6mm，5μm）色谱柱，流动相：甲醇-0．1％磷酸溶液（80：20）；检测波长：254mm；流速1．0ml·min^-1；柱温35℃。结果：大黄素在0．8—6．6μg·ml^-1（r=0．9999，n=5）范围内，有良好的线性关系，平均回收率为98．8％（n=9），RSD为1．7％。大黄酚在2．0—10．2μg·ml^-1（r=0．9999，n=5）范围内，有良好的线性关系，平均回收率为101．3％（n=9），RSD为1．6％。结论：方法具有操作简单、准确的优点，能有效控制祖卡木胶囊的质量。     

HPLC法同时测定复方乙胺嘧啶片中两组分的含量

目的：建立高效液相色谱法同时测定复方乙胺嘧啶片中两组分含量。方法：色谱柱Water C18（250mm×4．6mm，5μm），甲醇·水·三乙胺（40：55：5）为流动相，流速1．0ml·min，检测波长272nm。结果：乙胺嘧啶和氨苯砜的线性范围分别为6．4～22．6μg·ml^-1（r=0．9999）和32．4-113．6μg·ml^-1（r=0．9999），平均回收率分别为97．0％（RSD=0．9％）和100．3％（RSD=03％）。结论：方法简便、快速、准确可靠，适用于产品的含量测定。     

HPLC法测定乙胺吡嗪利福异烟片中4组分含量

目的：建立高效液相色谱法，测定乙胺吡嗪利福异烟片中利福平、异烟肼、吡嗪酰胺和盐酸乙胺丁醇含量。方法：利福平、异烟肼和吡嗪酰胺用C18色谱柱（150mm×4．6mm，5μm），以-0．01M磷酸二氢钾溶液-乙腈为流动相进行梯度洗脱，流速1．0ml·min^-1，检测波长254nm。盐酸乙胺丁醇选用C18色谱柱（150mm×4．6mm，5μm），四氢呋喃-0．4％庚烷磺酸钠（含有0．016％硫酸铜，用磷酸调pH至4．5）（25：75）为流动相，流速1．0ml·min^-1，检测波长258nm。结果：利福平、异烟肼、吡嗪酰胺及盐酸乙胺丁醇线性范围分别为16～160μg·ml^-1（r=0．9999），16—160μg·ml^-1（r=0．9999），53—532μg·ml^-1（r=0．9998），80～320μg·ml^-1（r=0．9998），平均回收率为99．3％～99．5％。结论：方法简便，准确，可用于乙胺吡嗪利福异烟片中各组分的质量控制。     

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.     

Efficacy of gut lavage,hemodialysis, and hemoperfusion in the therapy of paraquat or diquat intoxication

Clinical and in vitro investigations were carried out to test the efficacy of gut lavage, hemodialysis, and hemoperfusion in the treatment of poisoning with paraquat or diquat. In a patient suffering from diquat intoxication 130 times more diquat was removed by gut lavage 30 h after ingestion than was removed by complete aspiration of the gastric contents.Determination of in vitro clearances for paraquat and diquat by hemodialysis showed that, at serum concentrations of 1–2 ppm, such as are frequently encountered in poisoning in man, toxicologically relevant quantities of herbicide cannot be removed from the body. At a concentration of 20 ppm, on the other hand, hemodialysis proved to be effective, the clearance being 70 ml/min at a blood flow rate of 100 ml/min. The efficacy of hemoperfusion with coated activated charcoal was on the whole better. Especially at concentrations around 1–2 ppm, the clearance values for hemoperfusion were some 5–7 times higher than those for hemodialysis.In a patient suffering from paraquat poisoning, both hemodialysis as well as hemoperfusion were carried out. The in vitro results could be confirmed: At serum concentrations of paraquat less than 1 ppm no clearance could be obtained by hemodialysis while by hemoperfusion with activated charcoal quite high clearance values were measured and the serum level dropped down to zero.

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Zusammenfassung Klinische Untersuchungen und Laboratoriumsversuche wurden durchgeführt, um die Wirksamkeit von Darmspülung, Hämodialyse und Hämoperfusion bei Paraquat- und Deiquat-Vergiftungen zu prüfen.Bei einem Patienten wurde 30 Std nach Deiquat-Aufnahme durch Darmspülung 130mal mehr Deiquat entfernt als durch vollständige Aspiration des Mageninhaltes. In vitro-Versuche ergaben, daß bei Blutserumkonzentrationen von 1–2 ppm, die bei Vergiftungen oft gemessen werden, durch Hämodialyse keine toxikologisch relevanten Paraquat- oder Deiquat-Mengen entfernt werden können. Dagegen erwies sich die Hämodialyse bei 20 ppm und einer Blutumlaufgeschwindigkeit von 100 ml/min mit einer Clearance von 70 ml/min als wirksam. Die Hämoperfusion mit beschicheter Aktivkohle war in diesen Versuchen aber eindeutig überlegen, denn insbesondere bei Konzentrationen um 1–2 ppm waren die Clearance-Werte 5–7mal höher als bei der Hämodialyse.Die in vitro-Ergebnisse wurden bei einem Patienten mit einer Paraquat-Vergiftung bestätigt: Bei Konzentrationen unter 1 ppm war die Hämodialyse wirkungslos, während durch Hämoperfusion relativ hohe Clearance-Werte erreicht wurden, so daß der Serumspiegel rasch unter die Nachweisgrenze abfiel.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine.     

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.     

Steroidal sapogenin contents in some domestic plants

In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.