HPLC法测定卡瓦胡椒内酯的含量

目的 :建立测定 6种卡瓦胡椒内酯含量的HPLC法。方法 :采用硅胶色谱柱 ( 15cm× 3 9mm ,4μm) ,以正已烷 二烷( 82∶18,V/V)为流动相测定。结果 :去甲氧基醉椒素、二氢醉椒素、甲氧基醉椒素、醉椒素、二氢麻醉椒苦素、麻醉椒苦素 6种内酯依次在 0 10 4～ 2 0 8,0 10 9～ 2 18,0 117～ 2 3 4,0 12 6～ 2 5 2 ,0 10 2～ 2 0 4,0 113～ 0 2 6μg·mL-1范围内呈良好线性。加样回收率分别为 97 7% (RSD =1 6% ) ;99 0 % (RSD =1 9% ) ;96 8% (RSD =0 9% ) ;98 8% (RSD =1 0 % ) ;97 5 % (RSD =1 9% ) ;98 3 % (RSD =1 7% )。结论 :本方法可用于含卡瓦胡椒内酯药物的含量测定及质量控制     

HPLC测定小儿止泻颗粒中葛根素的含量

目的　采用高效液相色谱法测定小儿止泻颗粒中葛根素的含量。方法　固定相为HypersilC18柱 (4 .6mm× 15 0mm ,5μm) ;流动相为甲醇 -水 (2 3∶77) ;检测波长 2 5 0nm ;流速 1.0 0ml·min-1。结果　葛根素在 0 .2～ 1.0 μg·ml-1范围内 ,浓度与峰面积线性关系良好 (r=0 .9999) ,葛根素的加样回收率平均为 98.87% ,方法精密度RSD =2 .39%。结论　实验结果表明该方法准确、灵敏度高、重复性好     

HPLC法同时测定胃痛欣颗粒剂中大黄酸、大黄素、大黄酚的含量

目的建立胃痛欣颗粒剂中大黄酸、大黄素、大黄酚的含量测定方法。方法采用高效液相色谱法 ,AccusilC1 8(4 6mm× 2 5 0mm ,1 0 μm)柱 ,流动相为 :甲醇 水 冰醋酸 (80∶2 0∶1 ,V∶V∶V) ,检测波长为 2 5 4nm。结果大黄酸、大黄素、大黄酚分别在 0 0 3～ 0 4 8μg ,0 0 2 5～ 0 4 0 μg ,0 0 2 5～0 4 0 μg内与峰面积呈线性关系 ,平均回收率 (n =3 )分别为 98 3 % (RSD =1 4 3 % ) ,97 6% (RSD=1 84 ) ,98 7% (RSD =0 5 7% )。结论可用于大黄药材及其复方制剂的质量控制     

高效液相色谱法测定全血中葛根素含量

建立一种测定全血中葛根素浓度的HPLC方法。方法 :以Nova pakC18、4μm色谱柱为分离柱 ,以甲醇 水 (30∶70 )为流动相 ,采用HPLC法测定。结果 :全血中葛根素在浓度为 2～ 2 0 μg·ml-1范围内线性良好 (r =0 .9997) ,平均回收率为(97.1± 0 .8) % ,供试液日内RSD为 1.15 % ,日间RSD为 5 .2 7% ,最低检测浓度为 0 .1μg·ml-1。结论 :本文建立了一个可靠、简便的测定全血中葛根素的HPLC法。     

反相高效液相色谱法测定心安宁片中葛根素的含量

目的　建立心安宁片中葛根素含量测定的高效液相色谱法。方法　超声提取 ,色谱柱为Nova PakC18柱 (4μm ,15 0mm× 4 .0mm) ,流动相为甲醇 :水 (2 5∶75 ) ,检测波长为 2 5 0nm。结果　葛根素浓度在 8.2 6～ 4 1.30 μg·mL-1范围内与色谱峰面积呈良好的线性关系 (r =0 .9999)。平均加样回收率为 10 0 .15 % ,RSD =1.5 5 % (n =6 )。结论　本法简便 ,准确 ,灵敏度高 ,重现性好 ,可用于心安宁片中葛根素的含量测定。     

高效液相色谱法测定复方氯麻滴鼻液中三组分的含量

目的　建立高效液相色谱法测定复方氯麻滴鼻液含量的方法。方法　采用反相高效液相色谱法,以C18为固定相,甲醇0. 1mol·L-1醋酸铵溶液(磷酸调pH4. 0) (50∶50)为流动相,检测波长256nm。结果　氯霉素、盐酸麻黄碱和地塞米松磷酸钠的线性范围分别为: 12. 5~125μg·mL-1 (r=0. 999 4), 50~500μg·mL-1 (r=0. 9991)、2. 5~25μg·mL-1 (r=0. 9990)。平均加样回收率分别为99. 9% (RSD=1. 5% )、100. 3% (RSD=0. 7% ), 98. 7% (RSD=0. 9% )。结论　该方法简便、准确,适用于复方氯麻滴鼻液的质量控制。     

HPLC法测定天乐胶囊中的葛根素含量

目的 :建立了天乐胶囊中葛根素含量的测定方法。方法 :采用HPLC法 ,色谱柱为C18,柱温 4 0℃ ;流动相 :甲醇 0 5 %磷酸溶液 (2 0∶80V/V) ,流速 1 0mL·min-1;检测波长 2 5 0nm。结果 :线性范围 :2 9 2～ 14 6 0 μg·min-1,平均回收率 98 5 % ,RSD =0 78%。结论 :建立的定量方法可用于该品的质量控制     

HPLC法同时测定复方诺氟沙星滴鼻液中的诺氟沙星和盐酸麻黄碱

目的　建立一种快速、准确的高效液相色谱法同时测定诺氟沙星 ( NOR)和盐酸麻黄碱 ( EPH)的含量。 方法　使用 C1 8色谱柱 ,流动相为乙腈— 0 .1%磷酸 ( 15 :85 V/V) ,检测波长为 2 5 6nm。结果 　样品测定在 9min内完成。诺氟沙星在 10～ 60μg· ml- 1 浓度范围内 ,r=0 .9999,RSD= 0 .46% ,平均回收率为 99.91% ;盐酸麻黄碱在 2 5～ 12 5 μg· ml- 1浓度范围内 ,r=0 .9992 ,RSD=0 .5 1% ,平均回收率为 10 0 .0 3%。 结论 　方法可快速准确地检测复方诺氟沙星滴鼻液中的诺氟沙星和盐酸麻黄碱含量     

高效液相色谱法测定复方黄连颗粒中葛根素的含量

目的 :建立复方黄连颗粒中葛根素含量的测定方法。方法 :采用高效液相色谱法 ,色谱柱为C18(4 6mm×250mm ,5μm) ,检测波长为250nm ,流动相为甲醇 -水 (30∶70) ,流速为1 0ml/min ,柱温为30℃。结果 :葛根素在0 312μg～1 560μg范围内线性关系良好 (r=0 9989)。葛根素的平均回收率为99 2 % (RSD=2 08% ,n=5)。结论 :本方法具有灵敏度高 ,操作简单、稳定 ,分离效果好等优点 ,可作为复方黄连颗粒中葛根素的含量测定方法     

HPLC法同时测定白花蛇舌草中齐墩果酸和熊果酸的含量

目的建立同时测定白花蛇舌草中齐墩果酸和熊果酸含量的方法。方法采用HPLC法 ,色谱柱为HiQsilC18V (4 6mm× 15 0mm ,5 μm) (带预柱 ) ,流动相为甲醇 四丁基溴化铵(2 0mmol·L-1) 三乙胺 (V∶V∶V =90∶10∶0 0 2 ) (用冰醋酸调pH 6 9) ,检测波长 2 10nm ,流速0 3mL·min-1,进样量 2 0 μL。结果齐墩果酸和熊果酸分别在 9 80～ 15 6 8mg·L-1(r =0 9999)和 33 5～ 6 70mg·L-1(r =0 9999)内峰面积与质量浓度呈良好的线性关系 ;平均回收率 (n =9)分别为 98 3% (RSD =1 3% )和 98 0 % (RSD =1 4 % )。结论此方法可为不同产地白花蛇舌草中齐墩果酸和熊果酸的含量测定提供科学的依据     

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.