HPLC测定复方苯磺酸氨氯地平胶囊的含量

目的 采用HPLC法测定复方苯磺酸氨氯地平胶囊的含量.方法 采用Diamonsil C18色谱柱(150 mm×4.6 mm,5μm),流动相为甲醇-0.03 mol·L-1磷酸二氢钾溶液(75∶25),流速1.0 mL·min-1,检测波长238 nm.结果 苯磺酸左旋氨氯地平0.25～500 μg·mL-1与峰面积的线性关系良好(r=0.9999),平均回收率为99.6%(RSD=0.7%);辛伐他汀5.0μg·mL-1～1.0 mg·mL-1与峰面积的线性关系良好(r=0.9999),平均回收率为99.9%(RSD=0.6%).结论 所建方法准确、简便、快速,可用作复方苯磺酸氨氯地平胶囊的含量测定方法.     

双通道RP-HPLC法测定黄金搭档组合维生素片中VB1、VB2和VB6的含量

目的建立黄金搭档组合维生素片中维生素B1、B2和B6含量测定方法.方法用双通道反相高效液相色谱法进行分析.色谱柱为Lichrospher5-C18柱 ODS(5 μm,250 mm×4.6 mm),流动相为水-甲醇-0.25 mol*L-1庚烷磺酸钠溶液-乙酸-7%氨水(70:30:1.5:1:0.25),稀释液:同流动相,检测波长VB1248nm、VB2270 nm、VB6280 nm.结果峰面积与含量有良好的线性(γVB1=0.999920,γVB2=0.999993,γVB6=0.999 998);重复性好(批内RSDVB1=0.89%,RSDVB2=0.42%,RSDVB6=0.37%;批间RSDVB1=0.83%,RSDVB2=0.36%,RSDVB6=0.41%);回收率高(XVB199.3%,RSD=0.91%;XVB2100.1%,RSD=0.25%;XVB699.6%,RSD=0.46%).结论方法稳定,简便易行,快速准确,可作为此片剂质量检测方法.     

反相高效液相色谱法测定利福平滴眼液的含量

目的建立利福平滴眼液含量测定的分析方法。方法采用反相高效液相色谱(RP-HPLC)法测定利福平滴眼液中利福平的含量,色谱柱:HypersilC18柱(4.6mm×150.0mm,5μm);流动相:甲醇-乙腈-0.075mol.L-1磷酸二氢钾-1.0mol.L-1枸橼酸溶液(30∶30∶36∶4),流速:1mL.min-1,柱温:45℃,检测波长:254nm。结果利福平在20.14~161.12μg.mL-1的浓度范围内,线性关系良好(r=0.9999)。利福平平均回收率分别为98.9%(RSD=0.74%),100.7%(RSD=0.96%),98.7%(RSD=1.25%)。结论该法可用于测定利福平滴眼液中利福平的含量。     

反相高效液相色谱法测定地龙注射液中苯酚含量

目的建立反相高效液相色谱法测定地龙注射液中苯酚含量。方法采用反相高效液相色谱法,色谱柱:Waters C18色谱柱(4.6 mm×150 mm,5μm),流动相为甲醇-水(60∶40),柱温40℃,进样量20 L,检测波长254 nm。%HT5"H〗结果苯酚在0.002 0～0.020 0 mg.mL-1浓度范围内,线性关系良好,r=0.999(n=5);加样回收率99.46%,RSD=0.25%(n=9)。结论该方法简便,准确,重复性好,可用于该制剂的含量测定。     

HPLC法测定人用皮卡狂犬病疫苗和皮卡佐剂中硫酸卡那霉素的含量

目的:建立测定人用皮卡狂犬病疫苗和皮卡佐剂中硫酸卡那霉素含量的HPLC方法。方法:色谱柱为CAPCELL PAKC8 DD(4.6 mm×250 mm,5μm);流动相为磷酸二氢钾缓冲液(0.02 mol.L-1,pH 7.5)-甲醇-乙腈(23∶7∶40);流速为1.0mL.min-1;柱温为45℃;采用柱前衍生化法,衍生化试剂为2,4,6-三硝基苯磺酸(TNBS);检测波长为350 nm。结果:在0.01～1.0 mg.mL-1范围内,硫酸卡那霉素的浓度与峰面积呈现良好的线性关系(A=3×106C-3313.9,r=1.000,n=7);在80%,100%,120%3个浓度下的平均回收率(n=3)分别为82.5%(RSD=1.6%),90.3%(RSD=2.0%),81.6%(RSD=1.8%);方法的最低检测限为0.41μg.mL-1;最低定量限为1.39μg.mL-1;供试品溶液在8 h内稳定(RSD=1.1%)。结论:本方法准确、快速,通用性良好。     

高效液相色谱法测定炎琥宁注射剂的含量及有关物质

目的:建立高效液相色谱法测定炎琥宁针剂的含量。方法:使用HypersilC18柱(250mm×4.6mm,10μm),以0.05%磷酸二氢钾(pH3.0)-乙腈-甲醇(34∶4∶62)为流动相,流速为1.0mL.min-1,检测波长为251nm,柱温为30℃,测定炎琥宁针剂的含量。结果:该方法在0.119～3.808μg范围内峰面积与其浓度线性关系良好(r=0.9999);样品平均回收率为101.88%,RSD为1.21%(n=9)。日内精密度RSD为0.85%(n=5),日间精密度RSD为1.18%(n=5)。结论:该方法简便、准确可靠,可用作该制剂的含量测定及质量控制。     

RP-HPLC法测定接骨木中盐酸小檗碱的含量研究

目的采用反相高效液相色谱法建立接骨木中盐酸小檗碱含量的测定方法。方法采用反相高效液相色谱法,色谱柱:Hypersil ODS C18(4.6 mm×250 mm,5μm);流动相:甲醇-水-磷酸(25∶75∶0.2);柱温:30℃;检测波长:340 nm。结果盐酸小檗碱在4.90⁴9.0μg·mL-1范围内线性关系良好(r=0.999 8),精密度试验的RSD=0.36%,样品稳定性试验的RSD=1.08%,样品重复性试验的RSD=0.92%,平均回收率为98.68%(RSD=0.55%)。结论反相高效液相色谱法测定接骨木中盐酸小檗碱含量的方法简单、准确度高、重现性好,为制定接骨木的质量控制标准提供参考依据。     

高效液相色谱法测定联苯苄唑凝胶的含量

目的建立联苯苄唑凝胶质量标准的分析方法。方法采用高效液相色谱法(RP-HPLC)测定联苯苄唑凝胶中联苯苄唑的含量,色谱柱:Hypersil C18柱(4.6 mm×250 mm,5μm);流动相:甲醇-水-乙腈(80∶15∶5);流速1 mL.m in-1;柱温:40℃;检测波长:254 nm。结果联苯苄唑在12.56~125.60μg.mL-1的浓度范围内线性关系良好(r=0.999 9)。联苯苄唑平均回收率(n=3)分别为99.0%(RSD=0.74%),100.5%(RSD=0.96%),98.7%(RSD=0.55%)。结论该方法可以用于测定联苯苄唑凝胶中联苯苄唑的含量。     

HPLC测定乳块消分散片中橙皮苷的含量

目的建立乳块消分散片中橙皮苷的含量测定方法。方法采用HPLC法,色谱柱为Diamonsil C18(200 mm×4.6 mm,5μm),流动相为乙腈-水-磷酸(22∶78∶0.1),检测波长284 nm,流速1.0 ml.min-1,柱温40℃。结果橙皮苷的线性范围为14.95~598.00 ng(r=0.9999);平均回收率为99.0%,RSD=0.67%(n=5)。结论所用方法简便、快速、准确。     

HPLC法测定复方红景天胶囊中红景天苷和紫丁香苷的含量

目的:建立测定复方红景天胶囊中红景天苷和紫丁香苷含量的HPLC法。方法:采用Phenomenex C18(250 mm×4.6mm,10μm)色谱柱测定红景天苷的含量,流动相为甲醇-水(10∶55),流速1.0 mL.min-1,检测波长225 nm,柱温30℃;采用DiscoveryC18(250 mm×4.6 mm,5μm)色谱柱测定紫丁香苷的含量,流动相为乙腈(A)-水(B),梯度洗脱[0～35 min,A-B(6∶94);35～50 min,A-B(60∶40);50～60 min,A-B(6∶94)],流速1.0 mL.min-1,检测波长265 nm,柱温35℃。结果:红景天苷进样量在0.115～0.920μg(r=0.9999)范围内线性关系良好,平均回收率(n=5)为98.53%(RSD=1.1%);紫丁香苷进样量在0.0643～0.515μg(r=0.9999)范围内线性关系良好,平均回收率(n=5)为99.06%(RSD=0.74%)。结论:本方法操作简便,结果准确可靠,重复性好。     

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.