HPLC法测定复方罗布麻片Ⅰ中盐酸异丙嗪和氯氮(艹卓)的含量

目的:采用高效液相色谱法考察并建立了测定复方罗布麻片Ⅰ中盐酸异丙嗪和氯氮(艹卓)含量的方法.方法:色谱柱为Phenomenex-ODS3柱(250×4.60mm,5μm),甲醇-磷酸盐缓冲溶液(取磷酸二氢胺2.64g,加水1 000mL溶解后,用磷酸调节pH值至3.0)(55:45)为流动相,流速1.0mL/min,检测波长为250nm,进样量20μL.结果:盐酸异丙嗪的线性范围为5.1～60.8μg/mL(r=1.000 0),氯氮(艹卓)的线性范围为5.2～60.4μg/mL(r=0.999 9),平均回收率分别为99.5%和101.2%.结论:本法精密度好,结果准确可靠,适用于该复方制剂的质量检验分析.     

HPLC法测定复方罗布麻片I中盐酸异丙嗪和氯氮Zhuo的含量

目的采用高效液相色谱法考察并建立了测定复方罗布麻片Ⅰ中盐酸异丙嗪和氯氮(艹卓)含量的方法.方法色谱柱为Phenomenex-ODS3柱(250×4.60mm,5μm),甲醇-磷酸盐缓冲溶液(取磷酸二氢胺2.64g,加水1 000mL溶解后,用磷酸调节pH值至3.0)(5545)为流动相,流速1.0mL/min,检测波长为250nm,进样量20μL.结果盐酸异丙嗪的线性范围为5.1～60.8μg/mL(r=1.000 0),氯氮(艹卓)的线性范围为5.2～60.4μg/mL(r=0.999 9),平均回收率分别为99.5%和101.2%.结论本法精密度好,结果准确可靠,适用于该复方制剂的质量检验分析.     

HPLC法测定复方磷酸可待因糖浆主成分含量的研究

目的:建立测定复方磷酸可待因糖浆中磷酸可待因和盐酸异丙嗪的高效液相色谱方法。方法:采用氰基键合硅烷色谱柱为固定相,流动相为0.01 mol.L-1己烷磺酸钠溶液-乙腈-甲醇(54∶23∶23),流量1.0 mL.min-1,检测波长284 nm。结果:磷酸可待因的线性范围为0.3～2.8μg(r=0.9999),平均回收率为100.8%,定量限和检测限分别为10 ng和3 ng;盐酸异丙嗪的线性范围为0.2～1.9μg(r=0.9998),平均回收率为100.3%,定量限和检测限分别为6 ng和2 ng。结论:该方法简单、可靠,适用性好,可用于复方磷酸可待因糖浆的质量控制。     

HPLC法测定复方降压胶囊中氢氯噻嗪、地巴唑、氯氮(艹卓)和盐酸异丙嗪的含量

目的:建立离子对高效液相色谱法同时测定复方降压胶囊中氢氯噻嗪、地巴唑、氯氮(艹卓)和盐酸异丙嗪含量。方法:分析柱为 Hypersil C_(18)(4.6mm×250mm,5μm),流动相为乙腈-甲醇-7.2mmol·L~(-1)己烷磺酸钠溶液-冰醋酸-三乙胺(28∶28∶43∶1∶0.01),检测波长为258nm。结果:氢氯噻嗪、地巴唑、氯氮(艹卓)和盐酸异丙嗪的线性范围分别为12.24-122.4μg·mL~(-1)(r=0.9997),40.92-409.2μg·mL~(-1)(r=0.9998),8.12-81.2μg·mL~(-1)(r=0.9999),11.52-115.2μg·mL~(-1)(r=0.9999);平均回收率分别为100.3%(RSD<1.4%),99.0%(RSD<1.3%),98.8%(RSD<1.7%),99.4%(RSD<2.3%)。结论:4种组分分离效果好,其他组分和辅料无干扰,本法简便快速,准确可靠,适于该复方制剂中4种组分的同时测定。     

HPLC法测定复方止咳糖浆中盐酸异丙嗪和氢溴酸右美沙芬的含量

目的:建立高效液相色谱法,测定复方止咳糖浆中盐酸异丙嗪和氢溴酸右美沙芬的含量.方法:采用C18柱,以0.5%三乙胺溶液(用磷酸调节pH值至3.5)-乙腈(75:25)为流动相,检测波长为278nm.结果:线性范围为盐酸异丙嗪0.1738-0.8690μg(r=0.9999);氢溴酸右美沙芬0.447-2.235μg(r=1.0000),平均回收率为盐酸异丙嗪;100.0%(RSD%=0.87%,n=9);氢溴酸右美沙芬99.8%(RSD=0.3%,n=9).结论:本方法简便,快速,专属性强,可有效的控制复方止咳糖浆中盐酸异丙嗪和氢溴酸右美沙芬的含量.     

HPLC法同时检测氢氯噻嗪和盐酸可乐定

目的:采用高效液相色谱法同时测定氢氯噻嗪和盐酸可乐定。方法:phenomenex fusion-RP色谱柱(4.6mm×250mm,4μm);流动相:甲醇-水-磷酸(25:75:0.08);检测波长220nm;柱温25℃;流量1mL.min-1。氢氯噻嗪的检测灵敏度0.05AUFS,盐酸可乐定的检测灵敏度0.005AUFS。结果:氢氯噻嗪和盐酸可乐定的线性范围分别为20-400μg.mL-1(r=0.9999)和75~1500ng.mL-1(r=0.9999),平均回收率分别为99.3%和99.2%。结论:该法简便准确,可用于氢氯噻嗪和盐酸可乐定复方制剂含量的同时测定。     

RP-HPLC法测定复方明目汤中盐酸小檗碱的含量

目的建立测定复方明目汤中盐酸小檗碱含量的高效液相色谱法。方法色谱柱:Hypersil C18柱(250 mm×4.6 mm,5μm),流动相:乙腈-0.05 mol/L磷酸二氢钾溶液(45∶55),流速:1.0 mL/min,检测波长:265 nm。结果盐酸小檗碱的线性范围11.24~56.20μg/mL,r=0.999 9。平均回收率97.86%;RSD=1.42%。结论该法测定复方明目汤中盐酸小檗碱含量,操作简单,重复性好,精密度高。     

高效液相色谱法测定珍菊降压片中绿原酸、盐酸可乐定、氢氯噻嗪的含量及含量均匀度

目的建立高效液相色谱法测定珍菊降压片中盐酸可乐定、氢氯噻嗪的含量及含量均匀度。方法采用C18柱(250mm×4.6mm,5μm),测定盐酸可乐定的流动相为乙腈-0.2%磷酸(5∶95)、检测波长为210nm;测定氢氯噻嗪的流动相为甲醇-0.1%磷酸(15∶85),检测波长为332nm;流速1mL/m in。结果线性范围:盐酸可乐定7.132~142.64ng(r2=1.000 0);绿原酸0.0511~0.6132μg(r=0.999 9);氢氯噻嗪1.0023~12.0276μg(r=1.000 0)。加样回收率:盐酸可乐定为99.5%,RSD为2.7%(n=9);绿原酸为99.7%,RSD为1.57%(n=9);氢氯噻嗪为100.4%,RSD为1.03%(n=9)。结论本方法操作简单、结果准确,可作为控制本品质量的方法。     

复方利血平片中盐酸异丙嗪的含量测定及含量均匀度考察

目的建立测定复方利血平片中盐酸异丙嗪含量的高效液相色谱法。方法采用AgilentTCC18柱（250mm×4．6mm,5μm）,以乙腈-0．3％十二烷基硫酸钠溶液-磷酸（60：40：0．02．用三乙胺调pH至3．3）为流动相,流速为1．0mL／min,检测波长为250nm。结果盐酸异丙嗪进样量在0．504～1．176μg范围内与峰面积线性关系良好,r=0．9999（n=5）,平均回收率为98．71％,RSD=0．80％（n=9）。结论该法适用于复方利血平片中盐酸异丙嗪的含量测定。     

HPLC法同时测定复方可待因口服溶液中磷酸可待因、盐酸麻黄碱、盐酸曲普利啶的含量

目的 建立同时测定复方可待因口服溶液中磷酸可待因、盐酸麻黄碱、盐酸曲普利啶3组分含量的高效液相色谱法。方法 采用Hypersil-BDS CN柱,流动相为乙腈-0.4％乙酸铵溶液-三乙胺(30:70:0.2),流速为1.0 ml/min,检测波长257nm,外标法计算。结果 线性范围分别是磷酸可待因125-1 000 μg/ml,r=0.9999,盐酸麻黄碱75-600μg/ml,r=0.9996;盐酸曲普利啶18-140 μg/ml,r=0.9997。回收率分别为磷酸可待因99.9％、盐酸麻黄碱99.7％、盐酸曲普利啶100.3％。结论 本方法分离效果好,辅料无干扰,快速,简便,适合于该制剂3组分的同时测定。     

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.

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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.

     

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.     

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.     

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.     

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.