高效液相色谱法测定硝酸咪康唑栓的含量

目的建立测定硝酸咪康唑栓含量的高效液相色谱(HPLC)法。方法色谱柱为C18柱(150mm×4.6mm,5μm),流动相为甲醇-乙腈-0.5%乙酸铵(42.5∶42.5∶5),检测波长为230nm。结果硝酸咪康唑质量浓度在0.02～0.2mg/mL范围内与峰面积呈良好的线性关系(r=0.9999),平均回收率为101.3%,RSD为1.80%(n=9)。结论HPLC法准确、重现性好、简单,适用于硝酸咪康唑栓的含量测定。     

HPLC法测定复方硝酸咪康唑软膏中硝酸咪康唑和丙酸倍氯米松的含量

目的 建立高效液相色谱法同时测定复方硝酸咪康唑软膏中的硝酸咪康唑和丙酸倍氯米松的含量.方法 采用Hypersil ODS2 柱(4.6 mm×150 mm,5μm);流动相为0.5%醋酸铵∶甲醇∶乙腈(15∶42.5∶42.5);流速为1.0ml·min-1,检测波长240 nm.结果 硝酸咪康唑在0.976～2.278mg·mL-1范围岗位线性关系良好(r=0.9992),丙致倍氯米松在5.17～12.07μg·mL-1范围内线性关系良好(r=0.9997),硝酸咪康唑和丙酸倍氯米松的回收率分别为99.3%和98.7%.结论 本法快速、简便、准确,可有效地控制复方硝酸咪康唑软膏的质量.     

HPLC法测定归龙筋骨宁胶囊中士的宁含量

目的:建立归龙筋骨宁胶囊中士的宁的HPLC含量测定方法.方法:采用Thermo HTOERSIL Silica色谱柱(250mm×4.6mm,5μm),流动相为正己烷-二氯甲烷-甲醇-三乙胺(42.5:42.5:5.5:0.1),流速1.0ml/min,检测波长为254nm.结果:线性范围O.0660μg~0.6600μg(r=0.9999),呈良好线性关系,士的宁的平均加样回收率为99.38%,RSD=0.74%.结论:本方法操作简便,分离效果好,结果准确.     

高效液相色谱法测定百安洗液中盐酸小檗碱含量

目的建立百安洗液中盐酸小檗碱含量高效液相测定方法。方法色谱柱为Agilent Eclipse XDB-C18(5μm,4.6×150mm),流动相为乙腈-水-磷酸二氢钾-十二烷基磺酸钠(50∶50∶0.34∶0.17),流速1.0mL/min,测定波长为346nm。结果线性范围为0.0584~0.3504μg(r=0.9999),平均回收率为98.10%,RSD=1.66%(n=6),精密度RSD=1.23%(n=6),重复性RSD=1.82%(n=6)。结论方法简便、稳定、可靠,可用于百安洗液中盐酸小檗碱含量测定。     

RP-HPLC法测定黄金搭档组合维生素片中叶酸的含量

目的建立黄金搭档组合维生素片中叶酸含量测定方法。方法用反相高效液相色谱法进行分析。色谱柱为L ichro-spher-C18柱,ODS(5μm,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),检测波长280 nm。结果峰面积与含量有良好的线性(r=0.9997);重复性好(RSD=1.26%);回收率高(X=97.6%,RSD=1.95%)。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。     

RP-HPLC法测定硝酸咪康唑乳膏含量内外标比较

本文采用反相高效液相色谱内外标两种方法测定硝酸咪康唑乳膏的含量.固定相:ODS-C18;流动相:0.5%醋酸铵溶液-乙腈-甲醉(15∶42.5∶42.5);流速:1.0 ml·min-1;紫外检测波长:230 nm;内标法回收率100.44%,外标法回收率102.27%;两种方法的日内、日问相对标准偏差均小于2%.硝酸咪康唑的最低检测限为3ng,定量限为6ng;线性范围:0.3848～1.924 mg·mL-1,内标法r=0.9999;外标法r=0.9995.     

HPLC法测定硝酸咪康唑栓中硝酸咪康唑的含量

目的建立硝酸咪康唑栓的HPLC含量测定方法。方法采用HPLC法,色谱条件:ODS柱(250mm×4.6mm,5μm);甲醇-乙腈-5g.L-1醋酸铵溶液(42.5∶42.5∶15)为流动相;流速1.0mL.min-1;检测波长230nm;进样量10μL;柱温35℃。结果硝酸咪康唑进样量在0.499～2.994mg.mL-1范围内,其峰面积值与进样质量浓度有良好的线性关系,r=0.999 1,回收率为100.7%,RSD为1.0%(n=3)。结论经与紫外-可见分光光度法比较,该法重复性好,灵敏度高,结果准确,适用于硝酸咪康唑栓的含量测定。     

HPLC-ELSD测定肠外营养用海豹油脂肪乳中溶血磷脂酰胆碱的含量

目的建立HPLC-ELSD测定肠外营养用海豹油脂肪乳中溶血磷脂酰胆碱的含量。方法采用硅胶色谱柱(MZ-ANALYTICAL Spherisorb,250 mm×4.6 mm,5μm),流动相A为甲醇-水-冰醋酸-三乙胺(850∶1 50∶4.5∶0.5),流动相B为甲醇-水-冰醋酸-三乙胺-正己烷-异丙醇(385∶68∶2∶0.23∶1 60∶3 84),等度洗脱,A∶B=30∶70,流速为1.0mL.min1;进样体积为20μL,柱温为40℃;蒸发光散射检测器,漂移管温度为70℃,雾化气为氮气,气体流量为2 L.min1。结果线性范围为0.02~0.4 mg.mL1(r=0.999 4),检测限为0.12μg(S/N=3),定量限为0.40μg(S/N=10,n=3),平均回收率为100.3%,RSD为0.54%(n=9)。结论该方法灵敏、快速、准确、重复性好、专属性强,可用于本制剂的质量控制。     

不同显色剂对玉竹总皂苷含量测定的影响

目的:考察不同显色剂对紫外-可见分光光度法测定玉竹总皂苷含量的影响,确定最优显色方法。方法:采用紫外-可见分光光度法测定玉竹总皂苷含量,分别用三种显色剂,显色剂A为浓硫酸∶甲醇(4∶1),检测波长为405 nm;显色剂B为5%香草醛-冰乙酸∶高氯酸∶乙酸乙酯(2∶8∶10),检测波长为518 nm;显色剂C为5%香草醛-冰乙酸∶高氯酸∶冰乙酸(2∶8∶10),检测波长为518 nm。结果:采用方法C显色,玉竹总皂苷在6~36μg/mL范围内线性关系良好(r=0.999 9)。低、中、高3种浓度(0.4、0.5、0.6μg/mL)对照品溶液的日内RSD分别为1.05%、0.22%、1.20%(n=5),日间RSD分别为1.25%、1.08%、1.30%(n=5)。低、中、高3种浓度(0.34、0.39、0.44μg/mL)的加样回收率分别为(99.18±1.47)%、(100.32±0.72)%、(97.65±0.66)%(n=5);样品溶液在24 h内稳定。结论:方法C优于方法A和B,为最佳显色方法,重复性实验RSD最小,加样回收率和精密度最高,溶液稳定性最好。     

薄芝片的质量控制标准研究

目的:建立薄芝片的质量控制方法。方法:采用 TLC 方法,使用4%磷酸氢二钠的羧甲基纤维素钠溶液为粘合剂的硅胶 GF_(254)(10～40 μm)薄层板,以甲苯-乙酸乙酯-甲醇-异丙醇-浓氨试液(12∶6∶3∶3∶1)为展开剂,对薄芝片中核苷类成分腺苷进行定性鉴别;采用 HPLC 法,使用 Alltima C_(18)色谱柱(250 mm×4.6 mm,5 μm),以乙腈-水(5∶95)为流动相,流速1.0mL·min~(-1),检测波长262 nm,柱温25 ℃,进样量20 μL,对薄芝片中的腺苷和尿苷同时进行含量测定。结果:腺苷的 TLC 鉴别专属性强;HPLC 测定,腺苷、尿苷的线性范围分别为0.12～0.62μg(r=0.9994,n=5)和0.18～0.88μg(r=0.9998,n=5),平均回收率(n=6)分别为99.22%(RSD=2.2%)和100.5%(RSD=2.0%)。结论:本方法简单、可靠、准确,可用于控制薄芝片的质量。     

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.