反相高效液相色谱法测定补骨脂素和异补骨脂素的含量

目的:测定制斑素注射液中补骨脂素和异补骨脂素的含量.方法:采用反相高效液相色谱法,色谱柱为Spherisorb C18分析柱(150 mm×4.0 mm,5μm),流动相为甲醇-水(50∶60),紫外检测波长为295 nm,柱温为35℃,流速为1.1 mL/min.结果:补骨脂素浓度在10～90μg/mL(r=0.9999)范围内,异补骨脂素浓度在10～90μg/mL(r=0.999 8)范围内与峰面积呈线性关系;补骨脂素和异补骨脂素平均回收率(n=5)分别为98.52%(RSD=1.6%)和99.30%(RSD=1.6%).结论:反相高效液相色谱法操作简便、快速、准确、可行,可用于测定制斑素注射剂中补骨脂素和异补骨脂素的含量和该制剂的质量控制.     

反相高效液相色谱法测定补骨脂素和异补骨脂素钠含量

目的:测定制斑素注射液中补骨脂素和异补骨脂素的含量。方法:采用反相高效液相色谱法,色谱柱为SpherisorbC18分析柱(150mm×4.0mm,5μm),流动相为甲醇-水(5060),紫外检测波长为295nm,柱温为35℃,流速为1.1mL/min。结果:补骨脂素浓度在10～90μg/mL(r=0.9999)范围内,异补骨脂素浓度在10～90μg/mL(r=0.9998)范围内与峰面积呈线性关系;补骨脂素和异补骨脂素平均回收率(n=5)分别为98.52%(RSD=1.6%)和99.30%(RSD=1.6%)。结论:反相高效液相色谱法操作简便、快速、准确、可行,可用于测定制斑素注射剂中补骨脂素和异补骨脂素的含量和该制剂的质量控制。     

HPLC法测定克白酊中补骨脂素、异补骨脂素和盐酸异丙嗪的含量

目的建立高效液相色谱法(HPLC)测定克白酊中补骨脂素、异补骨脂素和盐酸异丙嗪的含量测定方法。方法采用HPLC对补骨脂素、异补骨脂素和盐酸异丙嗪的含量进行测定。结果克白酊中补骨脂素含量在10~100μg/ml范围内线性关系良好(r=0.9999),平均回收率99.0%(n=6),精密度RSD=0.13%;异补骨脂素含量在10~100μg/ml范围内线性关系良好(r=1),平均回收率99.6%(n=6),精密度RSD=0.10%;盐酸异丙嗪含量在10~80μg/ml范围内线性关系良好(r=0.9997),平均回收率101.1%(n=6),精密度RSD=2.04%。结论该方法简单,结果准确、重现性好,可作为该制剂的质量控制方法。     

HPLC法测定孕康糖浆中补骨脂素和异补骨脂素的含量

目的建立HPLC法测定孕康糖浆中补骨脂素和异补骨脂素含量的方法。方法采用高效液相色谱法测定。色谱柱:Agilent C18柱,流动相:甲醇-水(40∶60),流速:1.0 ml.min-1,检测波长:246 nm。结果补骨脂素在0.0334～0.334μg(r=0.9999),异补骨脂素在0.047 5～0.475μg(r=0.999 9)之间线性关系良好;补骨脂素的平均回收率为98.31%,RSD=1.49%;异补骨脂素的平均回收率97.30%,RSD=1.18%。结论试验表明,该方法操作简单,分离效果好,灵敏度高,可以用于孕康糖浆的质量控制。     

补骨脂微乳液中补骨脂素与异补骨脂素的含量测定

摘要目的建立高效液相色谱法测定补骨脂微乳液中补骨脂素和异补骨脂素的含量。方法采用Kromasil C18柱,以甲醇 0.6%醋酸溶液（50：50）为流动相,检测波长246 nm。结果补骨脂素在4.24～50.88 μg·mL－1浓度范围内呈良好的线性关系,平均回收率为99.3%（RSD＝1.51%）;异补骨脂素在4.48～53.76 μg·mL－1浓度范围内呈良好的线性关系,平均回收率为98.6%（RSD＝1.65%）。结论该方法简便可行,重复性好,可用于补骨脂微乳液中补骨脂素和异补骨脂素的含量测定。     

高效液相色谱法测定驱白巴布期片中补骨脂素和异补骨脂素的含量

目的建立驱白巴布期片中补骨脂素和异补骨脂素的含量测定方法。方法采用高效液相色谱法,色谱条件为:C18柱(4.6mm×150mm,5μm),流动相为乙腈-水(25∶75),流速1mL·min-1,检测波长为245nm,柱温为室温。结果补骨脂素、异补骨脂素浓度均在11~99mg·L-1范围内呈良好的线性关系;补骨脂素的平均回收率为99.86%,RSD为1.24%;异补骨脂素的平均回收率为100.01%,RSD为0.31%。结论该方法快速简便,结果准确,可用于驱白巴布期片的质量控制。     

高效液相色谱法测定万寿春口服液中补骨脂素和异补骨脂素的含量

采用高效液相色谱法测定了万寿春口服液中补骨脂素和异补骨脂素的含量。结果显示 ,补骨脂素对照品线性范围为2 .3 0～ 2 7.6ug,r=0 .9999,平均回收率为 99.2 % ,RSD=2 .0 % ;异补骨脂素对照品线性范围为 2 .0 6～ 2 4.7ug,r=0 .9999,平均回收率为 10 0 .3 % ,RSD=1.4%。     

反相高效液相色谱法测定 益宫宁血胶囊中补骨脂素与异补骨脂素的含量

［摘要］目的建立益宫宁血胶囊中补骨脂素和异补骨脂素的含量测定方法。方法采用反相高效液相色谱法，色谱柱为Diamonsil C18，流动相为甲醇 水 磷酸（53：47：0.2,V/V），流速为1.0 mL· min 1, UV检测波长为246 nm，柱温为25 ℃。结果补骨脂素和异补骨脂素的线性范围均为30～300 μg·mL 1，平均加样回收率分别为99.6%，RSD=1.45% 和 99.3%，RSD=1.15%（n=5）。结论该方法测定益宫宁血胶囊中补骨脂素和异补骨脂素的含量，简便、快捷、重现性好，可作为该产品的质量控制方法。     

高效液相色谱法测定驱白巴布期片中补骨脂素和异补骨脂素的含量

目的建立高效液相色谱法测定驱白巴布期片中补骨脂素和异补骨脂素的含量。方法高效液色谱法。Krom asil C18柱,乙腈-水(36∶64)为流动相,检测波长247nm。结果补骨脂素进样量在10~90ng,异补骨脂素进样量在9.6~86.4ng内线性关系良好,相关系数补骨脂素r=0.9999,异补骨脂素r=0.9999,平均回收率补骨脂素为99.87%(RSD=1.07%),异补骨脂素为98.70%(RSD=1.07%)。结论本法操作简便,结果准确,重现性好,可用于驱白巴布期片的质量控制。     

HPLC法测定生新发胶囊中补骨脂素和异补骨脂素含量

目的:建立同时测定生新发胶囊中补骨脂素和异补骨脂素含量的方法.方法:高效液相色谱法,色谱柱为Agilent TC-C18(250 mm×4.6 mm,5 μm),流动相为甲醇-水(46:54),流速为1.0 ml·min-1,检测波长为246 nm.结果:补骨脂素和异补骨脂素线性范围均为0.05~0.50 μg;平均加样回收率分别为100.11%,99.49%;RSD分别为1.12%,0.75%.结论:该方法准确、可靠、重复性好,能同时测定生新发胶囊中补骨脂素和异补骨脂素的含量,可作为生新发胶囊质量控制的含量检测方法.     

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.