高效液相色谱法同时测定白带净丸中的3'-羟基葛根素、葛根素、尿囊素、川续断皂苷Ⅵ和茯苓酸的含量

目的建立同时测定白带净丸中3'-羟基葛根素、葛根素、尿囊素、川续断皂苷Ⅵ和茯苓酸的HPLC法。方法采用Dikma-C_(18)(250 mm×4.6 mm,5μm),以乙腈(A)-0.5%磷酸溶液(B)为流动相,梯度洗脱,流速0.9 mL·min~(-1),柱温30℃,进样量为10μL。结果 3'-羟基葛根素、葛根素、尿囊素、川续断皂苷Ⅵ和茯苓酸的线性范围分别为:6.14~122.80μg·mL~(-1)(r=0.9993),7.59~151.80μg·mL~(-1)(r=0.9991),4.15~83.00μg·mL~(-1)(r=0.9999),8.13~162.60μg·mL~(-1)(r=0.9994),5.35~107.00μg·mL~(-1)(r=0.9997);平均回收率及RSD均符合药典规定。结论所建方法重复性好,专属性强,可用于白带净丸的质量控制。     

HPLC法同时测定康复新液中两种成分的含量

目的:建立同时测定康复新液中尿苷和黄嘌呤含量的方法。方法:采用HPLC法,Diamonsil C18(250mm×4.6 mm,5μm)色谱柱,甲醇-水(5:95)作为流动相,于254 nm波长下检测,流速1.0 mL·min~(-1),柱温30℃。结果:尿苷、黄嘌呤分别在0.10~3.96μg·mL~(-1)(r~2=0.9998)、0.52~20.80μg·mL~(-1)(r~2=0.9992)浓度范围内线性关系良好,平均加样回收率分别为97.86%(RSD=1.25%)、97.39%(RSD=0.68%)。测定5批次康复新液中尿苷和黄嘌呤的含量范围分别为1.69~1.76μg·mL~(-1)、12.76~13.06μg·mL~(-1),说明各批样品质量较均一。结论:本文建立的方法精密度高、重复性好,操作简便快速,可用于康复新液的质量控制。     

RP—HPLC法测定黄柏中小檗碱、巴马汀和药根碱的含量

目的:建立了用外标法对黄柏中小檗碱、巴马汀和药根碱同时定量的测定方法,考察小檗碱、巴马汀和药根碱的含量与其产地的关系。方法:高效液相色谱法,色谱柱:Kromasil-C_(18)(4.6mm×250mm,5μm),流动相:甲醇-乙腈-0.1mol·L~(-1)磷酸二氢钠(磷酸调pH为3.0)-2g·L~(-1)十二烷基硫酸钠-三乙胺(25∶25∶25∶25∶0.2),流速:1.0mL·min~(-1),检测波长:230nm,柱温:室温。结果:小檗碱、巴马汀和药根碱色谱峰面积与浓度呈良好的线性关系,线性范围分别是:盐酸小檗碱:21～495μg·mL~(-1),Y=3.144×10~6X 8.644×10~4,r=0.9999;盐酸巴马汀:2.0～40μg·mL~(-1),Y=7.570×10~5X 1.622×10~3,r=0.9999;盐酸药根碱:0.32～13μg·mL~(-1),Y=4.649×10~5X 2.161×10~3,r=0.9999。平均回收率小檗碱为98.0%,RSD为2.9%;巴马汀为97.7%,RSD为2.7%;药根碱为97.5%,RSD为2.4%。结论:本方法测定了21个不同产地的黄柏样品中小檗碱、巴马汀和药根碱含量,该方法分离度好,简便,重现性好。     

HPLC法测定维A酸与异维A酸含量

目的:建立HPLC法测定维A酸和异维A酸的含量方法。方法:采用Kromasil C_(18)(4.6mm×250mm,5μm)色谱柱,以甲醇-水-冰醋酸(90∶10∶0.5)为流动相,流速为1.0mL·min~(-1),柱温为30℃,检测波长为358nm。进样量20μL。结果:维A酸在4.4～17.4μg·mL~(-1)范围内线性关系良好,回归方程为A=8.127×10~3C 8.5698×10~2(r=0.9997),平均回收率为99.1%(RSD=0.7%)。异维A酸在1.083～4.332μg·mL~(-1)范围内线性关系良好,回归方程为A=103.73C 2.4(r=0.9999),平均回收率为100.1%(RSD=0.6%)。结论:该方法快速、准确,灵敏度高,重复性好,而且与其他降解产物能较好的分离。     

HPLC测定景天祛斑片中阿魏酸的含量

目的:建立 HPLC 方法测定景天祛斑片中阿魏酸的含量。方法:采用 CLC-ODS(6.0 mm×150 mm,5μm)色谱柱,以乙腈-0.1%磷酸(26:74)为流动相,流速0.8 mL·min~(-1),检测波长为323 nm,柱温30℃。结果:阿魏酸在2.4～24.0μg·mL~(-1)范围内呈良好的线性关系,回归方程为 Y=6.45×10~(-4)X 1.99×10~(-2),r=0.9999,平均加样回收率为98.6%,RSD=1.1%。结论:该方法简便,稳定准确,重现性好,能有效地控制该制剂的质量。     

HPLC测定风湿安泰片中马钱子碱和士的宁的含量

目的:采用反相高效液相色谱法测定风湿安泰片中士的宁和马钱子碱的含量。方法:采用 Hypersil BDS C_(18)色谱柱(4.6 mm×250 mm,5 μm),保护柱(4.6 mm×12 mm);乙腈-0.3%三乙胺溶液(磷酸调 pH=2.6)(10:90)为流动相,流速:1.0 mL·min~(-1),柱温:室温,检测波长:254 nm。结果:士的宁在4.6～46μg·mL~(-1)(r=0.9998),马钱子碱在2.65～26.5μg·mL~(-1)(r=0.9998)范围内呈良好的线性关系,士的宁的平均回收率(n=5)为101.1%,RSD 为2.8%;马钱子碱的平均回收率(n=5)为99.6%,RSD 为2.9%。结论:本方法准确、简便、快速,适用于风湿安泰片的质量控制。     

反相高效液相色谱法测定氢溴酸加兰他敏有关物质

目的:建立用反相高效液相色谱法测定氢溴酸加兰他敏有关物质。方法:色谱柱为十八烷基硅烷键合硅胶柱(250 mm×4.6 mm,5 μm),检测波长为228 nm,流动相为1%三乙胺溶液(磷酸溶液调 pH 值至6.0±0.1)-甲醇(75:25),流速为1 mL·min~(-1),柱温为30℃,进样鼍为10 μL。结果:加兰他敏、力克拉敏、表加兰他敏峰与相邻峰之间的分离度分别为5,6,5,分离良好。研究表明,在0.573～7.64μg·mL~(-1)范围内,氢溴酸加兰他敏线性关系良好,相关系数为1.000,n=5;在0.555～7.40μg·mL~(-1)范围内,氢溴酸力克拉敏线性关系良好,相关系数为1.000,n=5。氢溴酸加兰他敏、氢溴酸力克拉敏的检测限分别为1.9×10~(-10),6.2×10~(-10)g,定量限为11.4×10~(-10),18.6×10~(-10)g;在加样回收率实验中,3个浓度点9份杂质回收率结果的 RSD 均小于5%,回收率均大于95%。结论:本法简便准确,灵敏度高,适用于产品的质量控制。     

高效液相色谱法同时测定参菊洗剂中苦参碱和蛇床子素的含量

目的建立同时测定参菊洗剂中苦参碱和蛇床子素含量的方法。方法采用高效液相色谱法。色谱柱为Dionex C18(250mm×4.6mm,5μm),流动相为乙腈-2.4mL·L~(-1)三乙胺水溶液(用磷酸调pH至7.6),梯度洗脱,流速为1.0mL·min~(-1),检测波长为210nm,柱温为30℃,进样量为20μL。结果苦参碱和蛇床子素分别在30~192μg·mL~(-1)(r=0.999 5),4.4~70.4μg·mL~(-1)(r=0.999 5)范围内线性关系良好;平均回收率分别为99.4%和97.2%,RSD分别为1.4%和4.1%(n=9)。结论该方法简便、准确,可用于参菊洗剂的质量控制。     

天山地区红景天属植物根中红景天苷、苷元酪醇和百脉根苷的定量分析

目的:建立高效液相色谱方法测定天山地区红景天属植物根中红景天苷、苷元酪醇和百脉根苷的含量。方法:液相色谱分离系统采用岛津 VP5.0溶剂输送系统,LC10A TVP 自动进样器,PDA 检测器,色谱柱 VP-ODS 4 μm,150 mm×4.5mm,流动相为甲醇-乙腈-水(25:5:70),柱温40℃,分析时间15 min,检测波长275nm,进样量20μL。结果:方法简单、灵敏和精确。3物质的线性范围分别为:0.1714～2.2282 mg·mL~(-1)(r=0.9985),0.2012～2.6156 mg·mL~(-1)(r=0.9996)和0.1922～2.4986 mg·mL~(-1)(r=0.9994);回归方程分别为y=1.885×10~4 5.247×10~5X,Y=-1.284×10~4 7.077×10~5X 和 Y=-1.076×10~4 4.132×10~5X。结论:发现 Rhodiola rosea L.根中含有(44.38±0.7)mg·g~(-1)红景天苷,(16.37±0.9)mg·g~(-1)苷元酪醇和(8.06±0.7)mg·g~(-1)百脉根苷,并生长于相对较低海拔高度,认为是一个较具开发利用前景的目标植物。     

HPLC法测定儿童回春颗粒中哈巴苷和哈巴俄苷的含量

目的建立HPLC法同时测定儿童回春颗粒中哈巴苷和哈巴俄苷的含量。方法色谱柱为Kromasil C18(250mm×4.6mm,5μm);流动相为乙腈-0.3mL·L~(-1)磷酸溶液,梯度洗脱;流速:1.0mL·min~(-1);检测波长:210nm;进样量:10μL;柱温:25℃。结果哈巴苷与哈巴俄苷的线性范围分别为0.296~5.92μg·mL~(-1)(r=0.999 9)和0.103~2.06μg·mL~(-1)(r=0.999 8);平均回收率分别为99.3%(RSD=0.50%)和98.9%(RSD=0.72%)。结论该方法简便、准确、重复性好,可作为儿童回春颗粒的质量控制方法。     

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.     

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.