HPLC测定复方瓜子金颗粒中蒙花苷的含量

目的:采用HPLC法建立测定复方瓜子金颗粒中蒙花苷含量的方法。方法:色谱柱:SunFire C18柱(150 mm×4.6 mm,3.5μm),流动相:乙腈-水-冰醋酸(25∶73∶2),流速:1.0 ml.min-1,检测波长:334 nm。结果:蒙花苷在2.35～14.10μg.ml-1此浓度范围内线性关系良好,r=0.999 7,平均加样回收率为98.76%,RSD=0.38%。结论:该方法简便、可靠、准确,可用于复方瓜子金颗粒的含量测定。     

HPLC法测定复方五味子补肾颗粒中的五味子醇甲的含量

目的建立复方五味子补肾颗粒中五味子醇甲的含量测定方法。方法采用高效液相色谱法测定复方五味子补肾颗粒中五味子醇甲的含量。Welch Materials C18色谱柱(4.6 mm×250 mm,5μm);甲醇-水(70∶30)为流动相;流速:1.0 ml.min-1;柱温25℃。结果在高效液相色谱法图中,五味子醇甲与其它组份分离良好,线性范围为0.024 4～0.244 g.L-1,其回归方程为:Y=39 648.426X+51.18,r=0.999 9(n=6),线性良好为0.024 4～0.244 g.L-1,平均加样回收率为99.46%(RSD=0.54%)。结论该方法可以很好的用于控制复方五味子补肾颗粒的质量。     

复方天麻颗粒质量标准的研究

目的:建立复方天麻颗粒的质量标准。方法:采用薄层色谱法对方中五味子、麦冬进行鉴别。用高效液相色谱法对天麻中有效成分天麻素进行含量测定。色谱柱为 Kromasil-C_(18)柱(4.6 mm×250 mm,5 μm),柱温25℃;流动相为乙腈-0.05%磷酸溶液(2.5:97.5),流速1.0 mL·min~(-1);检测波长为220 nm。结果:薄层鉴别,色谱特征斑点明显;高效液相色谱法测定,天麻素在0.21～0.83 μg范围内线性关系良好(r=0.9999),平均回收率为98.2%(RSD=1.6%,n=6)。结论:本方法可有效地控制复方天麻颗粒的质量。     

高效液相色谱法测定复方金银花颗粒中黄芩苷的含量

目的 建立高效液相色谱法(HPLC)测定复方金银花颗粒中黄芩苷的含量.方法 色谱柱为Agilent HC-C18(4.6mm×250mm,5μm),流动相为甲醇-水-磷酸(44:56:1),检测波长为280nm,流速为1.0mL·min-1.结果 黄芩苷线性范围为12.176~608.8μg·mL-1(r=1.0000),平均回收率为99.39%(RSD=0.56%).结论 该方法 简便、快速、分离度好、结果 稳定,可用于复方金银花颗粒的质量控制.     

HPLC法同时测定通脉颗粒中丹参素、阿魏酸和葛根素的含量

目的:建立同时测定复方通脉颗粒中丹参素、阿魏酸和葛根素含量的方法。方法:采用高效液相色谱法测定。色谱柱为Agilent Zorbax SB-C18柱,流动相为乙腈-1%冰醋酸,流速为1.0mL·min-1。结果:丹参素、阿魏酸和葛根素的线性范围分别为2.95～29.5μg·mL-1(r=0.9999)、1.288～16.10μg·mL-1(r=0.9999)和5.26～52.6μg·mL-1(r=0.9997);平均加样回收率(n=6)分别为99.92%(RSD=1.53%)、100.0%(RSD=2.74%)和99.05%(RSD=1.46%)。结论:本方法简便、快速、可靠,可用于复方通脉颗粒的质量控制。     

HPLC法测定复方银连颗粒中绿原酸的含量

目的:建立测定复方银连颗粒中绿原酸含量的方法。方法:采用高效液相色谱法。色谱柱为Welchrom C18(250mm×4.6mm,5μm),流动相为乙腈-0.1%磷酸(10∶90),检测波长为327nm;流速为1.0mL·min-1,柱温为30℃。结果:绿原酸进样量在0.3035～1.5175μg范围内与峰面积积分值呈良好线性关系(r=0.9996);平均回收率为101.6%,RSD=1.84%(n=6)。结论:本方法操作简便、可靠,可用于复方银连颗粒的质量控制。     

HPLC法测定益母草药材、益母草颗粒及复方益母草膏中益母草碱的含量

目的:用HPLC测定益母草药材、益母草颗粒及复方益母草膏中的益母草碱的含量.方法:C_(18)色谱柱,流动相:甲醇-缓冲液(85:15),缓冲液为醋酸/醋酸钠的pH=1.7的缓冲溶液.流速0.6mL·min~(-1),检测波长277nm,灵敏度0.1AUFS,柱温25℃.结果:益母草药材、益母草颗粒及复方益母草膏中的益母草碱的含量为0.015%.2.4%、2.1%.结论:高效液相色谱检测益母草碱,简便易行,结果准确可靠,为益母草及其制剂的质量控制奠定了基础.     

RP-HPLC法测定复方自身清颗粒中马钱苷的含量

目的:建立以反相高效液相色谱法测定复方自身清颗粒中马钱苷含量的方法。方法:色谱柱为Agilent 1100 C18(250mm×4.6mm,5μm),流动相为乙腈-水(9.2∶90.8),流速为1.0mL·min-1,柱温为25℃,检测波长为240nm。结果:马钱苷的检测浓度在9～120μg·mL-1范围内与峰面积积分值呈良好的线性关系(r=0.9996);平均回收率为101.28%,RSD=1.74%(n=9)。结论:本方法简便、准确、可靠,可用于复方自身清颗粒的质量控制。     

HPLC法同时测定复方紫草颗粒中咖啡酸四聚体和丹酚酸B的含量

目的:建立以高效液相色谱法同时测定复方紫草颗粒中咖啡酸四聚体和丹酚酸B含量的方法。方法:色谱柱为YMC-PackODS-AC18(250mm×4.6mm,5μm),流动相为甲醇-0.5%磷酸水(40∶60),流速为1.0mL·min-1,检测波长为252nm,柱温为室温,进样量为10μL。结果:咖啡酸四聚体、丹酚酸B的进样量分别在0.065～1.82、0.205～5.74μg范围内与各自峰面积积分值呈良好的线性关系(r分别为0.9996、0.9997);平均回收率分别为98.72%(RSD=3.27%,n=9)、101.39%(RSD=1.81%,n=9)。结论:本方法简便、可靠、结果稳定、重复性好,可用于复方紫草颗粒的质量控制。关键词复方紫草颗粒;高效液相色谱法;咖啡酸四聚体;丹酚酸B;含量测定     

复方土茯苓颗粒定性定量方法研究

目的:建立复方土茯苓颗粒的定性定量方法。方法:采用TLC法对方中君药土茯苓、臣药牛膝进行定性鉴别;采用HPLC法测定方中牛膝的蜕皮甾酮,色谱柱为Agilent TC-18(250 mm×4.6 mm,5μm)柱,以水(A)-乙腈(B)为流动相梯度洗脱,流速1.0 mL.min-1,检测波长243 nm。结果:在TLC色谱中可检出土茯苓、牛膝;在HPLC色谱中,蜕皮甾酮可与其他成分分离,且在0.176~1.232μg范围内其峰面积与进样量呈良好的线性关系(r=0.9999,n=7),平均回收率为93.94%(RSD=1.1%,n=6)。结论:所建立的方法对方中的药材可准确、快速地进行定性、定量检测,可用于复方土茯苓颗粒的质量控制。     

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.