HPLC法同时测定瓜馥木药材中瓜馥木碱甲和duguevanine的含量

目的:采用反相高效液相色谱法测定瓜馥木药材中瓜馥木碱甲和duguevanine的含量。方法:使用Agilent ZORBAXSB-C18(250mm×4.6 mm,5μm)色谱柱,流动相为乙腈-0.05%磷酸二氢钾溶液(20∶80),流速1.0 mL.min-1,检测波长300nm。结果:瓜馥木碱甲、duguevanine进样量分别在0.019~0.372μg和0.009~0.184μg范围内,与峰面积呈良好线性关系;瓜馥木碱甲及duguevanine的平均回收率(n=6)分别为98.8%和99.1%,RSD分别为1.6%和1.9%。结论:本法简便、准确,重复性好,可为瓜馥木药材的质量控制提供实验依据。     

瓜馥木己素的化学结构研究

从广西瓜馥木茎皮的乙醇提取物中分到６个黄酮类成分，其中瓜馥木己素为新的双氢查耳酮，经各种波谱解析及Ｘ－晶体衍射分析，其结构鉴定为３，６－二羟基－２，４，５－三甲氧基双氢查耳酮。     

瓜馥木属植物化学成分研究概况

对瓜馥木属植物黄酮和生物碱等化学成分及其提取,分离和生物活性的研究进行了综述。     

HPLC法测定钻山风糖浆中芒柄花素的含量

目的:采用反相高效液相色谱法测定钻山风糖浆中芒柄花素的含量。方法:采用Diamonsil C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.5%磷酸(35∶65)为流动相,流速1.0 mL·min-1,检测波长248 nm,柱温30℃。结果:芒柄花素进样浓度在1.505～75.25μg·mL-1范围内,与峰面积呈良好线性关系;平均回收率(n=6)为98.6%,RSD为1.7%。结论:该方法简便、准确,重复性好,可作为钻山风糖浆质量控制方法。     

RP-HPLC法同时测定胃痛平糖浆中血根碱和小檗碱的含量

目的建立胃痛平糖浆的质量标准。方法采用高效液相色谱法对胃痛平糖浆中血根碱和小檗碱进行定量分析。色谱柱:Diamonsil C18色谱柱(250 mm×4.6 mm,5μm),流动相:乙腈-体积分数为1%的三乙胺水溶液(体积比为25∶75,三乙胺水溶液用磷酸调pH值3),流速:1 mL.min-1,检测波长:263 nm,柱温:30℃。结果血根碱和小檗碱的平均回收率分别为98.8%和99.7%。RSD分别为2.0%和1.7%。结论RP-HPL法可用于测定胃痛平糖浆中血根碱和小檗碱的含量。     

HPLC测定钻山风总生物碱的含量

目的建立高效液相色谱法测定钻山风总生物碱的含量。方法采用高效液相色谱法,以C₁₈(250 mm×4.6 mm,5 μm)为色谱柱,以0.1 mol·L^-1磷酸二氢钠溶液(用2.0 mol·L^-1氢氧化钠溶液调节pH至6.00±0.05)-乙腈为流动相,流速为1.0 mL·min^-1,柱温为室温,检测波长为277 nm,进样量为20 μL。结果钻山风总生物碱的主要成份为牛耳枫碱、木番荔枝碱分别在10.0～50.0和8.0～40.0 μg·mL^-1内呈线性关系。牛耳枫碱平均回收率为98.7%,RSD为0.93%。木番荔枝碱平均回收率为99.0%,RSD为0.54%。结论方法结果准确,适用于钻山风总生物碱的含量测定。     

高效液相色谱法测定清咽糖浆中盐酸小檗碱的含量

目的:建立清咽糖浆中盐酸小檗碱含量的高效液相色谱法。方法:色谱柱为Zorbax Ec lipse XDB-C8(4.6mm×150mm,5μm);流动相为0.05mol.L-1磷酸二氢钾(三乙胺调pH至8.0)-乙腈(77∶23),检测波长346nm;柱温30℃;流速1.0mL.m in-1。结果:盐酸小檗碱在31.5~756ng(r=0.999 8,n=6)范围内呈良好的线性关系;平均回收率为87.16%,日内RSD为0.16%(n=5),日间RSD为0.68%(n=5)。结论:本法检测快速,定量准确,可用于清咽糖浆的定量分析。     

HPLC法测定柘木糖浆中山柰酚的含量

目的:建立测定柘木糖浆中山柰酚含量的方法。方法:采用高效液相色谱法。色谱柱为CalesilODS-100C18(250mm×4.6mm,5μm),流动相为甲醇-0.2%乙酸溶液(梯度洗脱),流速为1mL.min-1,检测波长为360nm。结果:山柰酚进样浓度在1～50μg.mL-1范围内与峰面积积分值呈良好的线性关系(r=0.9998);平均加样回收率为99.77%,RSD=1.21%(n=9)。结论:本方法快速、简便、专属性强,可用于柘木糖浆的质量控制。     

ELSD-HPLC测定馥感啉口服液中贝母素甲的含量

目的采用ELSD-HPLC法测定馥感啉口服液中贝母素甲的含量。方法采用C18柱(250mm×4.6mm,5μm),以乙腈-水-二乙胺(70∶30∶0.3)为流动相,蒸发光散射检测器检测。结果浙贝母素甲在0.522～5.220μg范围内线性关系良好;平均回收率为101.8%,RSD为3.9%。结论该方法简便、灵敏、准确、重复性好,可作为控制馥感啉口服液质量的一种方法。     

HPLC测定钻山风总生物碱的含量

目的建立高效液相色谱法测定钻山风总生物碱的含量。方法采用高效液相色谱法,以C18(250 mm×4.6 mm,5 μm)为色谱柱,以0.1 mol·L-1磷酸二氢钠溶液(用2.0 mol·L-1氢氧化钠溶液调节pH至6.00±0.05)-乙腈为流动相,流速为1.0 mL·min-1,柱温为室温,检测波长为277 nm,进样量为20 μL。结果钻山风总生物碱的主要成份为牛耳枫碱、木番荔枝碱分别在10.0～50.0和8.0～40.0 μg·mL-1内呈线性关系。牛耳枫碱平均回收率为98.7%,RSD为0.93%。木番荔枝碱平均回收率为99.0%,RSD为0.54%。结论方法结果准确,适用于钻山风总生物碱的含量测定。     

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.

---

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.