HPLC测定扎西他宾薄膜衣片的溶出度

目的 建立定量测定扎西他宾薄膜衣片溶出度的方法. 方法采用HPLC法,AlphaBond-C18柱 (150 mm×3.9 mm,10 μm),流动相为磷酸缓冲液-甲醇-乙腈(96:4:3),检测波长270 nm. 结果 0.005～20.000 μg·ml-1的线性方程为:A＝4.455×105C 1.770×104 (r＝0.9999);平均回收率为99.28%,RSD＝0.83% (n＝9);5批样品溶出迅速,批间差异小. 结论所建方法简单,专属性强,可测定扎西他宾薄膜衣片的溶出度.自制片剂和进口参比制剂溶出度相似.     

HPLC法测定氯诺昔康口腔崩解片的含量

目的:建立HPLC法测氯诺昔康口腔崩解片的含量。方法:色谱柱为,Linksil C18(4.6mm×250mm,5μm),流动相为0.05mol·L-1磷酸二氢钾溶液(用磷酸调pH值至3.1)-乙腈-甲醇(60∶30∶10),流速为1.0ml·min-1;检测波长为264nm;柱温为40℃。结果:氯诺昔康的线性范围为4.0~60.0mg·L-1,r=0.9998;平均回收率为99.8%,RSD=0.63%。结论:本方法方便、快速、准确,可用于该制剂的质量控制。     

HPLC法测定盐酸噻诺啡片的含量及其溶出度

目的:建立一种HPLC法测定盐酸噻诺啡片的含量及溶出度.方法:采用Phenex prodigy C18色谱柱(250mm×4.6mm,5μm),以乙腈-甲醇-0.02mol·L-1磷酸盐缓冲液(pH=3,含0.2%的三乙胺)(40:15:45)为流动相,220nm为检测波长,测定了盐酸噻诺啡片的含量和溶出度.结果:本法测定盐酸噻诺啡的线性范围为0.5～10μg·mL-1(r=0.999 9);日内精密度和日间精密度均小于2%(n=5);回收率在98%～102%之间.结论:本法精密、准确,适用于盐酸噻诺啡片的含量及溶出度测定.     

高效液相色谱法测定氯诺昔康速释片的含量

目的建立了氯诺昔康速释片含量的HPLC测定法。方法采用C18色谱柱,柱温35℃,流动相为0.1mol·L-1醋酸钠溶液-甲醇(1∶1),检测波长为378nm。结果氯诺昔康在9.5μg·mL~285.5μg·mL范围内线性良好,相关系数r=1.0000(n=5);平均回收率为99.69%(n=6,RSD为0.9%)。结论HPLC法可以测定氯诺昔康速释片的含量。     

氯诺昔康口腔崩解片的质量控制

目的:建立氯诺昔康口腔崩解片的质量控制方法。方法:利用自制崩解装置测定氯诺昔康口腔崩解片的崩解时限;以紫外-可见分光光度法测定溶出度;采用高效液相色谱法进行含量测定。结果:氯诺昔康口腔崩解片的崩解时间不超过20s,标示含量达到99.2%以上,10min内溶出度在90%以上。结论:建立的质量控制方法简便可靠,可用于该制剂的质量控制。     

高效液相色谱法测定氟氯西林钠片的溶出度

目的:建立氟氯西林钠片溶出度的测定方法.方法:高效液相色谱法,色谱柱为Hypersil BDS C18柱(200mm×4.6mm, 5μm),流动相为0.02mol·L-1磷酸二氢钾缓冲液(用稀NaOH调节pH至5.0)-乙腈(70:30),检测波长为225nm,流速为1.0ml·min-1,柱温为25℃.照中国药典2005年版二部附录"溶出度测定法"第二法测定溶出度.结果:3批样品溶出量均为标示量的94%.结论:该法简便、准确,结果可靠.可用于氟氯西林钠片的溶出度测定.     

紫外-可见分光光度法测定氯诺昔康颗粒的溶出度

目的: 建立测定氯诺昔康颗粒溶出度的方法。方法: 照《中国药典》2010年版二部溶出度测定第二法,以磷酸盐缓冲液(pH 7.4)900 mL为溶出介质,转速50 rpm,15 min取样,用紫外-可见分光光度法测定溶出量,检测波长为376 nm。结果: 氯诺昔康在1.105～22.100 g·L^-1浓度范围内吸光度线性关系良好(r=0.999 9,n=5),平均回收率为99.7%(RSD=0.63%)。结论: 本方法简便,准确可靠,能满足质量控制的要求。     

氯诺昔康口腔崩解片的制备

目的:对氯诺昔康口腔崩解片的处方及制备工艺进行研究,并评价其质量。方法:以片剂崩解时限、口感为指标,采用正交试验设计优化处方。通过直接压片法制备氯诺昔康口腔崩解片,并测定了其体外崩解时间、溶出度等质量指标。结果:所得片剂完整光洁、口感良好,能在20 s内崩解完全,5 min内体外溶出度超过85%。结论:氯诺昔康口腔崩解片达到了设计要求,方便患者服药。     

炔诺酮片溶出度测定方法学研究

目的建立炔诺酮片溶出度检查方法。方法采用桨法进行溶出度实验,高效液相色谱法测定介质中药物含量。结果溶出度检查方法为桨法,以5g.L-1十二烷基硫酸钠溶液500mL为溶出介质,转速为75r.min-1,取样时间为45min(薄膜衣片)或60min(糖衣片)。含量测定方法的线性方程为Y=64 743 X-208(r=1.000 0),在0.12～1.84μg.mL-1质量浓度范围内线性关系良好(r=1.000);A企业样品平均回收率为100.1%,RSD为1.3%,B企业样品平均回收率为100.8%,RSD为0.7%。结论该方法准确可靠,适用于该制剂的质量控制。     

紫外分光光度法测定氯诺昔康注射液的含量

目的 采用分光光度法测定氯诺昔康注射液的含量。方法 以水为溶媒，测定波长378nm的条件下，对氯诺昔康注射液进行含量测定，另外还对样品的测定条件进行了优选。结果 氯诺昔康浓度在4μg-20μg范围内线性良好，以标准曲线法得其回收率为99.7%(n=5),RSD为0.78%。结论 该方法稳定可靠，重现性好，辅料及杂质无干扰。     

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.     

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.