HPLC测定银杏叶中聚戊烯醇的含量

目的建立测定银杏叶中聚戊烯醇含量的方法。方法采用HPLC法,色谱柱为Kromasil ODS柱(250 mm×4.6 mm,5μm),流动相为异丙醇-甲醇-正己烷-水(50∶25∶15∶2),流速0.9 ml.min-1,柱温27℃,检测波长210 nm。结果在1.08~2.88μg.ml-1范围内,聚戊烯醇浓度与峰面积呈良好的线性关系(r=0.9979)。平均回收率为96.8%(RSD<2%,n=3)。结论所建方法快速、准确、稳定,为银杏叶中聚戊烯醇含量测定提供了可靠的方法。     

正交设计法在银杏叶聚戊烯醇提取工艺中的应用

目的从银杏叶中提取聚戊烯醇同系物并对其提取工艺进行优化。方法用正交试验法以聚戊烯醇得率为指标对提取工艺进行优化,经硅胶柱色谱纯化,用高效液相色谱法(HPLC)测定聚戊烯醇含量。结果银杏聚戊烯醇提取工艺的最佳条件为以用7倍体积石油醚索氏提取10 h。结论优选出银杏聚戊烯醇提取工艺,验证试验符合要求。     

中药材木通质量评价方法的研究

目的:建立TLC和HPLC法,同时对木通中齐墩果酸和常春藤皂苷元进行定性、定量分析。方法:薄层鉴别采用硅胶G薄层板,展开剂:正己烷-醋酸乙酯-冰醋酸(6:4:0.25),显色剂:10％硫酸乙醇溶液;含量测定采用Kromasil C18色谱柱(4.6mm×150 mm,5 μm),流动相:甲醇-水-冰醋酸-三乙胺(87:13:0.04:0.02),检测波长:210 nm,流速:0.8 mL·min-1,柱温:室温。结果:TLC色谱系统中,齐墩果酸与常春藤皂苷元分离效果良好;HPLC中齐墩果酸、常春藤皂苷元线性范围分别为2.03-50.8μg(r=0.9996)和2.08-52.1μg(r=0.9997),平均回收率(n=5)分别为99.1％(RSD=1.8％)和97.4％(RSD=2.0％)。结论:所建立的TLC和HPLC法重现性好,专属性强,为木通药材质量控制提供科学依据。     

高效液相色谱法测定松龄血脉康胶囊中葛根素的含量

目的建立HPLC法测定松龄血脉康胶囊中葛根素的含量。方法以Ultrasphere-ODS(4.6mm×250mm,5μm)色谱柱为分离柱,流动相甲醇-水（25∶75),检测波长245nm。结果葛根素在0.534～10.68μg.ml     

银杏叶提取物及其制剂中非法添加染料木素的检测

目的：对银杏叶提取物及其制剂中非法添加染料木素进行鉴定和检测。方法：采用HPLC-DAD法,色谱柱为DIKMA Inertsil ODS-3 (4.6mm×250mm,5μm),流动相为甲醇-0.4%磷酸溶液(50:50),流量1.0ml?min-1,柱温35℃,检测波长260nm,并同时采集210～400nm的光谱图,对银杏叶、银杏叶提取物及其制剂中的染料木素进行定性分析。结果：部分银杏叶提取物和银杏叶制剂样品HPLC色谱图中出现与染料木素对照品保留时间一致的色谱峰,DAD光谱一致。结论：部分厂家生产的银杏叶提取物及其制剂中含有染料木素,为生产时添加了其他含染料木素的原料。     

高效液相色谱法测定氯霉素滴眼液中氯霉素的含量

目的:建立一种简便快速的分析氯霉素滴眼液的方法。方法:应用高效液相色谱法(HPLC),采用ZorbaxSB-C18柱(5μm,4.6mm×250mm),以甲醇-水(60∶40)为流动相,检测波长为314nm。结果:氯霉素浓度在10～100μg/mL范围内与峰面积线性关系良好,平均回收率为99.0%,RSD为1.16%(n=6)。结论:HPLC法简便快速,测量结果可靠。     

不同产地白芷药材HPLC指纹图谱的研究

目的:采用RP-HPLC法对12个产地的白芷药材进行指纹图谱的研究,并与其混淆品兴安白芷进行比较。方法: 95％乙醇溶液回流1 h提取,色谱柱为岛津ULTRON VX-ODS(4.6 mm×250 mm,5μm)柱,流动相为甲醇-水-冰乙酸(60: 40:1),流速0.8 ml/min,检测波长254 nm。结果:本研究所建立的分析方法有较好的重现性。结论:12个白芷样品HPLC指 纹图谱地域差异不明显。     

高效液相色谱法测定盐酸班布特罗片的含量

采用HPLC法测定盐酸班布特罗片的含量,色谱柱为ODS(150 mm×4.6mm,ID,4μm),流动相为甲醇-乙腈-50mmol/L辛烷磺酸钠-磷酸缓冲液(34:11:55),检测波长为214 nm,线性范围为10～100μg/ml,平均回收率为99.1l％,相对标准偏差为0.59％。     

大孔吸附树脂在测定阳春口服液的淫羊藿甙中的应用

为排除干扰性成分,准确、快速地用HPLC法测定阳春口服液中淫羊藿甙的含量。采用大孔吸附树脂(DA-201)吸附样品,以水、15％乙醇洗脱除去干扰成分,以70％乙醇洗脱液用于HPLC测定。用ID4.6mm×250mm Hypersil ODS柱,以甲醇-水(50:50)为流动相,在270nm波长处测定。回归方程Y=1.826×10⁵X—7.771×10²,r=0.9996(n=5);平均回收率为98.22％(n=5),RSD=0.66％(n=5)。精密度RSD=2     

HPLC法测定硝呋拉呔的含量及有关物质的方法学研究

目的:采用高效液相色谱法测定硝呋拉呔的含量及有关物质。方法:采用ODSC_(18)色谱柱(5μm,4.6mm×250mm),以甲醇-水(45:55)为流动相,流速1.2 mL·min~(-1),紫外检测器于254 nm测定。结果:HPLC法测定的线性范围为0.01～0.4mg·mL~(-1),r=0.999 9,最低检测限0.2 ng;样品溶液在8 h内稳定,日内精密度和日间精密度(RSD<1.0％)良好。回收率为100.1％。结论:采用HPLC法测定硝呋拉呔及有关物质的方法简便,结果可靠。     

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.     

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.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

Abstract

The uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors.