高效液相色谱法测定盐酸氯丙嗪注射液的含量

目的 采用高效液相色谱测定盐酸氯丙嗪注射液的含量.方法 采用C18(4.6 mumx 250 mm5 μm)色谱柱;流动相:0.1 mol/L磷酸二氢钾(用磷酸调节pH 3.0)-乙腈(55∶45);检测波长254 nm;流速:1.0 ml/min;进样量:20μl;柱温:35℃.结果 在该色谱条件下,盐酸氯丙嗪在4.99～49.91μl/ml范围内呈良好的线性关系,(r =0.9999,n=8).结论 所建立的方法灵敏、准确、简便,可作为盐酸氯丙嗪注射液的含量测定方法.     

HPLC-蒸发光散射检测器法测定丙泊酚注射液中大豆油的含量

目的:建立高效液相色谱-蒸发光散射检测器法测定丙泊酚注射液中大豆油含量的方法。方法:色谱柱为硅胶柱;以正己烷-异丙醇-冰醋酸(98.9∶1∶0.1)为流动相;流速为1.0ml/min;蒸发光散射检测器(ELSD);空气泵压力2.0L/min;检测器温度40℃;进样量10μl。结果:测得大豆油的回收率为99.99%,RSD为2.4%;进样量在0.951-2.853μg范围时,线性方程为Y=1.4282X 4.5912,r=0.999。结论:方法快速简便,结果准确。     

右旋糖酐-40葡萄糖注射液中葡萄糖的含量测定

目的:建立右旋糖酐-40葡萄糖注射液中葡萄糖含量的高效液相色谱测定法。方法:采用高效液相色谱法,色谱柱采用磺化交联苯乙烯-二乙烯共聚合物的氢型阳离子交换树脂为填充剂(300 mm×7.8 mm);流速为0.6 m L/min;柱温为40℃;采用示差折光检测器检测,进样量为20μL。结果:葡萄糖浓度在1~10 mg/m L范围内呈良好的线性关系,葡萄糖的平均回收率为102.23%(RSD=0.70%,n=9),测得右旋糖酐-40葡萄糖注射液中葡萄糖含量平均为51.33 mg/m L。结论:本方法灵敏度高、操作简单、准确可靠,适用于高效液相色谱法测定右旋糖酐-40葡萄糖注射液中葡萄糖的含量。     

HPLC法测定二氮嗪注射液的含量

目的:建立测定二氮嗪注射液含量的方法。方法:采用高效液相色谱法。色谱柱为Waters symmetry-C18,流动相为0.01mol/L庚烷磺酸钠-甲醇-醋酸(79∶20∶1,V/V/V),检测波长为254 nm,流速为1.0 ml/min,柱温为30℃,进样量为20μl。结果:二氮嗪的质量浓度在30~110.0μg/ml范围内与峰面积呈良好线性关系(r=0.999 8);精密度、稳定性、重复性试验的RSD<1.0%;加样回收率为99.57%,RSD=0.94%(n=3)。结论:本方法简便、准确,专属性好,精密度高,可用于二氮嗪注射液的质量控制。     

HPLC法测定依托咪酯脂肪乳注射液中依托咪酯的含量

目的建立测定依托咪酯脂肪乳注射液中依托咪酯含量的高效液相色谱法。方法色谱柱:Agilent TC-C18柱(250mm×4.6mm,5μm),流动相∶甲醇-水(80∶20),流速1.0mL/min,检测波长:241nm,进样量:20μL。结果依托咪酯的浓度在5～50μg/mL范围内与峰面积呈良好线性关系(r=0.9990),高、中、低3种浓度的平均回收率(n=3)为99.3%(RSD=0.11%)、98.1%(RSD=0.08%)、100.3%(RSD=0.14%)。结论该方法操作简便,结果可靠,适用于依托咪酯脂肪乳注射液的含量测定。     

RP-HPLC法测定盐酸乌拉地尔注射液含量和有关物质

目的:建立高效液相色谱方法测定盐酸乌拉地尔注射液的含量和有关物质。方法:采用C18色谱柱(4.6 mm×250 mm,5μm);流动相为乙腈-0.1 mol/L磷酸二氢铵缓冲液-三乙胺(15∶85∶0.2,磷酸调pH值6.0);柱温:35℃;检测波长:270 nm;流速:1.0 ml/min;进样量:20μl。结果:盐酸乌拉地尔注射液在10~30μg/ml范围内线性关系良好;回归方程为:A=162 412 182 121C,r=1.000(n=5);最低检测限为0.02 ng;平均加样回收率为99.84%(n=9),RSD为0.35%。结论:该方法简便灵敏、结果准确可靠,可用于该制剂的含量测定及有关物质检查。     

高效液相色谱法测定安乃近氯丙嗪注射液中盐酸氯丙嗪含量

目的 采用高效液相色谱法测定安乃近氯丙嗪注射液的含量.方法 采用C18色谱柱(250 mm×4.6 mm,5μm),流动相为0·1 mol/L磷酸二氢钾(用磷酸调节pH:3.0)-乙腈(55:45),检测波长254 nm,流速1.0 mL/min,进样量20μL,柱温35℃.结果 盐酸氯丙嗪质量浓度在4.99-49.91μg/mL范围内与峰面积呈良好线性关系,r=0.9999(n=8).结论 所建立的方法灵敏、准确、简便,可作为安乃近氯丙嗪注射液的含量测定方法.     

RP-HPLC法测定穿心莲注射液中苯甲醇的含量

目的:建立测定穿心莲注射液中苯甲醇含量的方法。方法:采用反相高效液相色谱法。色谱柱为Kromasil C18(250mm×4.6mm,5μm),流动相为乙腈-水(35∶65),流速为0.5mL·min-1,检测波长为210nm,柱温为40℃,进样量为20μL。结果:苯甲醇检测浓度在0.595～11.900μg·mL-1范围内与峰面积积分值呈良好线性关系(r=0.9999);平均加样回收率为99.0%,RSD=0.7%(n=9)。结论:本方法简便、准确、重复性好,可用于穿心莲注射液的质量控制。     

HPLC法测定阿魏酸钠注射液含量

目的应用高效液相色谱法测定阿魏酸钠注射液含量。方法本品采用Phenomenex色谱柱(250mm×4.6mm,5μm),甲醇-水-冰乙酸(69∶30∶1.5)为流动相,流速为1.0mL.min-1,检测波长为322nm。结果阿魏酸钠在0.07196~0.86352mg.mL-1范围内峰面积与进样量呈良好的线性关系,r=0.9999。结论该分析方法结果准确,重复性好,可用于阿魏酸钠注射液的质量控制。     

高效液相色谱法测定丹墨胶囊中丹酚酸B含量

目的建立测定色谱丹墨胶囊中丹酚酸B含量的高效液相色谱法。方法色谱柱为Ecosil C18柱(200 mm×4.6 mm,5μm),流动相为乙腈-甲醇-甲酸-水(10∶30∶1∶59),检测波长286 nm。结果丹酚酸B进样量在0.120 042～2.400 84μg范围内与峰面积呈良好的线性关系,平均回收率为103.40%,RSD为0.70%(n=6)。结论该方法简便、灵敏、准确,可用于丹墨胶囊的质量控制。     

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.     

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.