RP-HPLC测定注射用复方甘草酸苷中甘草酸铵含量和有关物质

目的:采用高效液相色谱法测定注射用复方甘草酸苷中甘草酸铵的含量和有关物质。方法:采用 Symmetry C_(18)色谱柱(4.6 mm×250 mm,5 μm),以2%醋酸-乙腈(65:35)为流动相,流速为1.0 mL·min~(-1),检测波长为256 nm,进样量为20μL。结果:甘草酸铵线性范围为40～400μg·mL~(-1)(r=0.9999),最小检测量为6.23 ng。结论:本法精密度好,结果准确、可靠、灵敏,可用于注射用复方甘草酸苷含量测定和有关物质检查。     

HPLC法测定阿普唑仑片的含量及含量均匀度

目的建立HPLC法测定阿普唑仑的含量及含量均匀度。方法采用日本岛津VP-ODS色谱柱(250mm×4.6mm,5μm),以甲醇-水(65∶35)为流动相,检测波长254nm,流速:0.7mL.min-1,柱温:30℃,进样量:10μL。结果阿普唑仑线性范围为8.96～89.6μg.mL-1(r=0.9996),平均回收率为99.7%(RSD=1.2%)。结论本方法灵敏度高,操作简便、可靠,适用于阿普唑仑片的质量控制。     

HPLC法测定兰索拉唑片含量及有关物质

建立高效液相色谱法测定兰索拉唑片含量及有关物质的方法。方法采用C18色谱柱(4.6mm×250mm,5μm),以水-乙睛-三乙胺(60∶40∶1)用磷酸调pH7.0为流动相,流速:1.0mL.min-1,检测波长为285nm,进样量20μL,柱温35℃。结果兰索拉唑浓度在19.76~177.84μg.mL-1时,其峰面积与浓度的线性关系良好(r=1);平均回收率为99.6%,平均相对标准偏差RSD为0.5%;检测限为0.02ng.mL-1。结论本法快速、简便、准确,灵敏度高,适用于兰索拉唑片含量及有关物质测定。     

HPLC同时测定腰痛宁贴片中的士的宁和马钱子碱

目的 采用RP-HPLC法同时测定腰痛宁贴片中士的宁和马钱子碱的含量.方法 采用Inertsil C8色谱柱(250 mm×4.6 mm,5 μm),流动相为甲醇-水-冰醋酸(100:480:35,三乙胺调pH3.2),流速1.0 mL·min-1,检测波长254 nm,柱温30℃,进样量10μL.结果 士的宁和马钱子...     

HPLC法测定盐酸莫西沙星中R-异构体含量

目的:建立HPLC法对盐酸莫西沙星S-和R-异构体进行拆分并测定其中R-异构体含量。方法:采用AD-H手性柱(DAICEL CHIRALPAK,250 mm×4.6 mm,5μm),流动相为正己烷-异丙醇-二乙胺-乙酸(85∶15∶0.2∶0.1),流速1.0 mL.min-1,柱温35℃,检测波长293 nm;进样量10μL。结果:盐酸莫西沙星异构体之间的分离度为3.4,R-异构体的线性范围为0.54～5.40μg.mL-1(r=0.9995),检测限为1.1 ng,平均回收率(n=9)为99.2%。结论:该方法操作简便,结果准确,可用于盐酸莫西沙星中R-异构体含量测定。     

HPLC法测定复方红景天胶囊中红景天苷和紫丁香苷的含量

目的:建立测定复方红景天胶囊中红景天苷和紫丁香苷含量的HPLC法。方法:采用Phenomenex C18(250 mm×4.6mm,10μm)色谱柱测定红景天苷的含量,流动相为甲醇-水(10∶55),流速1.0 mL.min-1,检测波长225 nm,柱温30℃;采用DiscoveryC18(250 mm×4.6 mm,5μm)色谱柱测定紫丁香苷的含量,流动相为乙腈(A)-水(B),梯度洗脱[0～35 min,A-B(6∶94);35～50 min,A-B(60∶40);50～60 min,A-B(6∶94)],流速1.0 mL.min-1,检测波长265 nm,柱温35℃。结果:红景天苷进样量在0.115～0.920μg(r=0.9999)范围内线性关系良好,平均回收率(n=5)为98.53%(RSD=1.1%);紫丁香苷进样量在0.0643～0.515μg(r=0.9999)范围内线性关系良好,平均回收率(n=5)为99.06%(RSD=0.74%)。结论:本方法操作简便,结果准确可靠,重复性好。     

HPLC法测定生骨胶囊中丹酚酸B的含量

目的:建立用高效液相色谱法测定生骨胶囊中丹酚酸B含量的方法.方法:采用Agilent-C18色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-甲酸-水(35∶1∶64),柱温为28℃,流速为1.0 ml·min-1,检测波长为286 nm.结果:丹酚酸B进样量在0.096 ～1.435μg范围内与峰面积线性关系良好,平均回收率为101.6％,RSD为0.7％(n=9).结论:所用方法简便、快捷、准确,可作为生骨胶囊中丹酚酸B的含量测定方法.     

HPLC法测定蒙成药三子散中没食子酸的含量

目的:建立蒙成药三子散中没食子酸的含量测定方法.方法:采用HPLC法,采用Phenomenex C18色谱柱(250mm×4.6 mm,5μm),流动相为甲醇-0.1％磷酸水溶液(5:95),流速1.0 mL(min-1,柱温35℃,进样量为10μL,检测波长为273nm.结果:没食子酸进样量范围在6.357～158....     

高效液相色谱法测定安乃近氯丙嗪注射液中盐酸氯丙嗪含量

目的 采用高效液相色谱法测定安乃近氯丙嗪注射液的含量.方法 采用C18色谱柱(250 mm×4.6 mm,5μm),流动相为0·1 mol/L磷酸二氢钾(用磷酸调节pH:3.0)-乙腈(55:45),检测波长254 nm,流速1.0 mL/min,进样量20μL,柱温35℃.结果 盐酸氯丙嗪质量浓度在4.99-49.91μg/mL范围内与峰面积呈良好线性关系,r=0.9999(n=8).结论 所建立的方法灵敏、准确、简便,可作为安乃近氯丙嗪注射液的含量测定方法.     

HPLC法测定肾康丸中大黄酚、大黄素的含量

目的:建立肾康丸中大黄酚、大黄素的含量测定方法。方法:采用HPLC法,色谱柱为Diamonsi C18(250 mm×4.6 mm,5μm),流动相为乙腈-甲醇-0.1%磷酸溶液(42∶23∶35),流速为1.0 ml.min-1,检测波长为254 nm,进样量10μl。结果:大黄酚在9.38～150.00μg.ml-1(r=1.000 0),大黄素在3.31～53.00μg.ml-1(r=1.000 0)之间线性关系良好,其平均加样回收率大黄酚为99.83%,RSD为0.75%;大黄素为99.73%,RSD为0.34%。结论:此法简便,结果准确、灵敏,可用于肾康丸的含量测定。     

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.

     

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.     

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.     

Gender-related symptoms and correlates of alcohol dependence among men and women with a lifetime diagnosis of alcohol use disorders

This study explored gender-related symptoms and correlates of alcohol dependence in a crosssectional study of 150 men and 150 women with a lifetime diagnosis of alcohol use disorders (AUD). Participants were recruited in equal numbers from treatment settings, correctional centres and the general community. Standardized measures were used to determine participants' use of substances, history of psychiatric disorders and psychosocial stress, their sensation seeking and family history of substance use and mental health disorders. Multivariate analyses were used to detect patterns of variables associated with gender and the lifetime severity of AUD. Men had a longer history of severe AUD than women. Women had similar levels of alcohol dependence and medical and psychological sequelae as men, despite 6 fewer years of AUD. More women than men had a history of severe psychosocial stress, severe dependence on other substances and antecedent mental health problems, especially mood and anxiety disorders. There were differences in family history of alcohol-related problems approximating same-gender aggregation. The severity of a lifetime AUD was predicted by its earlier age at onset and the occurrence of other disorders, especially anxiety, among both men and women. The limitations in the generalizability of these findings due to sample idiosyncrasies are discussed.     

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.