头孢拉定中三种有关物质的表面增强拉曼光谱研究

摘 要 目的:研究头孢拉定中三种有关物质的拉曼光谱及表面增强拉曼光谱, 对三种目标物在不同酸碱条件下的表面增强拉曼光谱进行分析。方法: 用便携式拉曼光谱仪对三种物质的常规拉曼光谱与不同酸碱条件下的表面增强拉曼光谱进行考察,并参照头孢拉定有关物质与主成分实际比例模拟实验,测定了不同条件下头孢拉定的有关物质。 结果: 三种物质均能在表面增强拉曼光谱中表现出跟常规拉曼光谱相对应的特征峰信息,酸碱度对于三种物质表面增强拉曼光谱的检测均有一定的影响。在体系偏酸性的条件下可实现头孢氨苄与7 氨基去乙酰氧基头孢烷酸的同时检出,偏碱性的条件下光谱表现为头孢氨苄的特征峰;而双氢苯甘氨酸在两种pH条件下的光谱特征性都不明显。结论: 头孢拉定有关物质的表面增强拉曼光谱体现出一定的指纹性特征,可用表面增强拉曼光谱对头孢拉定有关物质进行初步鉴别。     

TLC-SERS同时检测银黄软胶囊中3种非法添加成分

目的 建立薄层色谱-表面增强拉曼光谱（TLC-SERS）联用技术同时检测中成药银黄软胶囊中非法添加的西药化学成分双氯芬酸钠、芬布芬、盐酸罗通定。方法 将待测样品点于硅胶板,用石油醚-乙酸乙酯（3:5）进行薄层展开,在254 nm紫外光灯下进行定位检测,在分离的各个斑点处按优选的最佳条件喷加纳米银胶溶液,用表面增强拉曼光谱（SERS）进行定性鉴别。结果 本研究建立了TLC-SERS联用技术同时检测银黄软胶囊中非法添加的双氯芬酸钠、芬布芬、盐酸罗通定的方法,并确定了3种化学成分的最低检测限。结论 TLC-SERS联用技术快速、准确、灵敏度高,可同时快速检测银黄软胶囊中非法添加的双氯芬酸钠、芬布芬和盐酸罗通定3种成分。     

左氧氟沙星的拉曼光谱研究

摘 要 目的:研究左氧氟沙星的固体常规拉曼光谱及表面增强拉曼光谱,对其分子振动模式进行识别。方法: 采用便携式拉曼光谱仪对左氧氟沙星的常规拉曼和表面增强拉曼进行考察,并对几种左氧氟沙星注射剂进行了表面增强拉曼光谱检测。结果:在表面增强拉曼光谱中,左氧氟沙星的几个特征峰明显增强,可很好地识别左氧氟沙星的几种注射剂。结论:该方法简单、快速、可靠、专属性强,可以用作鉴别左氧氟沙星。     

红花注射液表面增强拉曼光谱研究

摘 要 目的： 研究红花的表面增强拉曼光谱,利用表面增强拉曼光谱技术对红花注射液进行快速有效的鉴别。 方法: 通过对红花注射液图谱与相应对照药材标准图谱的比较分析,实现对红花注射液的快速鉴别。结果:研究表明,红花的几个特征峰在表面增强拉曼光谱中得到了很明显的增强,表面增强拉曼光谱可很好地识别红花注射液。结论: 该方法简单、快速、可靠、专属性强,可以作为鉴别红花及红花注射液的方法。     

药物辅料中有毒掺杂物的拉曼/近红外光谱法检测灵敏度评价

目的 建立常用药物辅料(甘油)中有毒掺杂物(二甘醇)的快速检测方法。 方法 利用拉曼/近红外光谱法结合移动窗口相关系数法评价有毒掺杂物的检测灵敏度。 结果 拉曼光谱下获得的检测灵敏度优于近红外光谱,同时移动窗口法可进一步提高检测灵敏度。 结论 拉曼光谱法有望成为现场快速检测药物辅料中掺杂有毒物质的有效方法。     

基于整体柱的表面增强拉曼光谱法检测非法染色青黛

目的 建立基于整体柱的表面增强拉曼光谱(surface enhanced Raman spectroscopy, SERS)法快速检测非法染色的青黛。 方法 采用混合溶剂乙醇-水(1:1,V/V)对染色青黛中的染料进行提取,利用整体柱中网状孔隙有助于银纳米颗粒在空间上耦合的特性,将样品溶液和银胶溶液混匀后滴加于整体柱上进行SERS光谱采集。 结果 此法可得到青黛中染色掺伪量低至500 μg/kg的孔雀石绿SERS信号。 结论 该方法具有快速、简便、专属性强等优点,可运用于中药材青黛非法染色的快速检测。     

薄层色谱-表面增强拉曼光谱法快速检测染色掺伪的西红花

目的 建立一种薄层色谱-表面增强拉曼光谱法对染色掺伪的西红花进行检测。方法 将乙醇溶液润湿的西红花按压在表面喷有银溶胶的薄层板上,然后对按压区域进行表面增强拉曼散射（SERS）检测。依次对润湿剂的浓度、银溶胶的喷洒时间和喷洒量等因素进行优化。结果 成功检测经金胺O、新品红、柠檬黄和胭脂红4种常见染料染色的西红花药材。结论 薄层色谱-表面增强拉曼光谱法可实现对染色西红花简单、快速、灵敏的检测要求,并满足现场快速检测的需求。     

头孢氨苄与相似化合物头孢羟氨苄的拉曼光谱比较

摘 要 目的:比较分析头孢氨苄及其相似化合物头孢羟氨苄的拉曼光谱,对结构特征相关性进行分析和探讨。方法: 采用傅里叶拉曼光谱仪、显微拉曼光谱仪及便携式拉曼光谱仪对头孢氨苄进行光谱检测,并对相似化合物头孢羟氨苄进行了傅立叶拉曼光谱检测。结果:在3台不同的拉曼仪的3种不同的激发光光源的激发下,头孢氨苄的大部分特征峰的峰位基本一致,但相对峰强却有区别;头孢氨苄与头孢羟氨苄的傅立叶拉曼光谱存在一定的差异,体现了化学结构差异与拉曼光谱差异的相关性。结论:拉曼光谱相对峰强的差异反映了激发光对不同基团或骨架结构的选择性激发。该法简单、快速、可靠、专属性强,可实现自动识别,对样品无损,有望成为药品日常监督中一种有效的鉴别手段。     

人参、红参、西洋参3种配方颗粒的傅里叶变换红外光谱快速鉴别方法

目的 建立人参、红参、西洋参3种配方颗粒的傅里叶变换红外光谱快速鉴别方法。方法 采用红外光谱及其二阶导数光谱、二维相关光谱,分析不同配方颗粒的红外光谱特征。结果 傅里叶变换红外光谱能够从整体上反映化学成分的不同情况,二阶导数光谱和二维相关光谱在800~1800 cm^-1能够对不同配方颗粒进行不同程度的区分,二维相关光谱的区分效果明显。结论 通过综合比较傅里叶变换红外光谱、二阶导数光谱和二维相关光谱,可以准确、快速鉴别人参、红参、西洋参3种配方颗粒。     

应用近红外光谱和拉曼光谱建立主成分分析模式识别法鉴别不同厂家阿法骨化醇软胶囊

摘 要 目的：比较近红外光谱法和拉曼光谱法对不同厂家阿法骨化醇软胶囊进行模式识别的特点,建立定性模型,并对不同厂家的阿法骨化醇软胶囊进行分析鉴别。方法: 应用近红外光谱与拉曼光谱,首次采用主成分分析的模式识别方法,结合光谱信息分析处方工艺,对不同厂家的阿法骨化醇软胶囊进行近红外光谱和拉曼光谱分析。结果: 近红外光谱法与拉曼光谱法均能提取出阿法骨化醇软胶囊的光谱信息,并进行判别分析。制剂中不同着色剂的荧光效应的影响在拉曼光谱中体现出较大差异。据此,建立了拉曼光谱主成分分析判别模型,前三个主成分重构的三维图中,代表6个不同厂家来源的阿法骨化醇样品点各自聚集,相互区分,实现了正确判别。结论: 利用拉曼光谱与近红外光谱互补性,建立不同工艺的阿法骨化醇软胶囊的识别方法,可用于阿法骨化醇软胶囊工艺一致性的分析。     

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.     

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.