HPLC测定肝速康胶囊中齐墩果酸的含量

肝速康胶囊为《卫生部药品标准中药成方制剂》第十三册收载的品种,由齐墩果酸粗品和云芝多糖两味药组成,本品具有降酶,降浊,调整机体免疫功能,改善代谢障碍、肝病症状及加速肝功能恢复等作用,临床上用于急、慢性、迁延性肝炎。本实验以方中主要活性成分齐墩果酸为测定指标,采用高效液相色谱法测定其含量,并经方法学考察,认为本法可行,为该制剂的质量控制提供了快速、准确的测定方法。1仪器与试药仪器:PU-1580高压液相泵,日本JASCO公司UV-1575紫外检测仪,CK色谱王工作站。试药与试剂:齐墩果酸对照品批号为709-9803(中国药品生物制品检定…     

双氯芬酸钠肠溶片的血药浓度测定及人体药代动力学研究

目的 :研究双氯芬酸在正常志愿者的血药浓度及体内的药代动力学 ,为临床用药提供依据。方法 :16名健康男性志愿者 ,单剂量口服双氯芬酸钠肠溶片 10 0 mg,在不同时间点取静脉血 ,血药浓度采用高效液相色谱法 (HPL C)测定。由血药浓度数据获得各自的主要药动力学参数。结果 :志愿者单次服用 10 0 mg双氯芬酸钠肠溶片后的药代动力学参数 AUC0→∞ 、AU C0→ 8、Cmax、Tmax分别为 (5 .98± 1.4 7) mg.h/ L、(6 .15± 1.5 2 ) mg.h/ L、(2 .96± 0 .84 ) m g.h/ L、(2 .2 5± 0 .32 ) h。结论 :双氯芬酸钠肠溶片在我国正常志愿者的药代动力学参数与国外的相似。     

地高辛的体内分析方法应用与进展

目的总结地高辛血药质量浓度监测方法,寻求最适的测定方法。方法对近年来国内外与地高辛监测相关的文献进行检索综述分析。结果地高辛血药浓度测定方法很多,常用方法主要有:FPIA、酶免疫分析法、RIA、CLIA、乳胶免疫抑制法、干化学法、HPLC法等。结论通过比较分析其中RIA、CLIA、EIA和HPLC MS 4种方法更好。     

HPLC法测定盐酸美沙酮含量

本文采用高效液相色谱法，以盐酸布比卡因为内标，检测波长220nm，在Symmetry-C18柱上，以己腈-磷酸二氢钾（pH2．5）（3862，V／V）为流动相，测定盐酸美沙酮及其口服液的含量。方法平均回收率为100．17％，日内及日间的RSD均＜1％。方法简便、快速、准确。     

反相高效液相色谱法测定洛氟沙星的血药浓度

采用反相ＨＰＬＣ法测定洛氟沙星的血药浓度，血浆样品用二氯甲烷在ｐＨ７．０条件下提取后进样，流动相为１０ｍ ｍｏｌ／Ｌ磷酸二氢钾－１０ｍ ｍｏｌ／Ｌ溴化四丁铵－乙腈－三乙胺（４５：４４：１０：１，磷酸调节ｐＨ２．８），紫外检测器λ＝２９５ｎｍ，最低检测浓度１０μｇ／Ｌ，线性范围：０．１￣６．０ｍｇ／Ｌ，ｒ＝０．９９９９，日内ＲＳＤ为１．３８％￣３．４２％，日间ＲＳＤ为１．１１％￣２．８９％。     

双氯芬酸钠滴眼液稳定性研究

采用高效液相色谱法测定双氯芬酸钠滴眼液的含量，方法简便，准确，能将药与杂质峰完全分离。应用化学动力学原理以恒温加试验预测双氯芬酸钠滴眼液稳定性及有效期，室温下有效期ｔ＾２５℃０．９约为２．５７年，与留样观察结果相符。     

关于单结合胆红素水溶性的研究

目的:进一步研究单结合胆红素(MCB)的水难溶特性及其在病理性胆汁中参与胆红素沉淀和色素性结石形成的作用机制.方法:应用胆红素高效液相色谱分析技术,先从人胆汁中获得结合胆红素,再经分离、制备及纯化得到纯MCB.然后观察其水溶解度并与其它型胆红素比较.结果:在pH7.9,温度37℃接近生理的条件下,MCB的溶解度(558.25±5.96μm)仅为双结合胆红素(DCB)的1/7,比不结合胆红素(UCB)高约44倍并随pH值改变而呈曲线变化.pH7.9时最大;pH4.5时为0;而当pH>9时,反而低于呈离于状态的UCB.结论:MCB虽作为结合型胆红素在胆道生理条件下的不溶性明显高于UCB,但比DCB要低得多;而在胆道病理条件下,其水溶性不但远低于DCB,甚至还不如离子化的UCB,这可能是MCB参与胆红素沉淀及胆色素结石形成的理化基础.     

A new and highly sensitive method for measuring 3-methoxytyramine using HPLC with electrochemical detection. Studies with drugs which alter dopamine metabolism in the brain

3-Methoxytyramine (3-MT) is a minor metabolite of dopamine which is suggested to reflect the turnover and utilization of dopamine. A novel, isocratic HPLC method has been developed which can be used to analyse 3-MT in homogenates of rat brain without the need for additional purification procedures. Furthermore, the coulometric electrochemical detection system is sensitive enough to measure 3 pg of 3-MT (equivalent to 0.6 ng/g tissue wet weight). 3-Methoxytyramine was measured in the striatum and n. accumbens after decapitation and rapid freezing, using 3-methoxy-4-hydroxybenzylamine as the internal standard. The effects of dopaminergic and other drugs on this metabolite were examined using this method. -Methyl-p-tyrosine (200 mg/kg i.v.) produced parallel linear decreases in dopamine and 3-MT in naive rats, but not those pretreated with tranylcypromine (5 mg/kg i.p.). Methamphetamine (0.3–10 mg/kg i.p.) and amphetamine (0.3–10 mg/kg i.p.) both dose-dependently increased 3-MT in naive and tranylcypromine-pretreated rats. In naive animals, 3-MT was not altered by intraperitoneal injection of the dopamine reuptake inhibitors, bupropion (10 mg/kg) and nomifensine (10 mg/kg) or by sibutramine HCl (3 mg/kg), amitriptyline (10 mg/kg), desipramine (10 mg/kg) and zimeldine (10 mg/kg). 3-Methoxy-tyramine was decreased by apomorphine (5 mg/kg i.p.) and also by large doses of the selective D₂ antagonist, BRL 34778 (5 mg/kg i.p.) or -DOPA (50 mg/kg i.p.). The selective D₁ antagonist, SCH 23390 (0.1 or 5 mg/kg i.p.) was without effect. In tranylcypromine-pretreated rats, 3-MT was dose-dependently reduced and increased by apomorphine (0.01–5 mg/kg i.p.) and BRL 34778 (0.1–5 mg/kg i.p.), respectively. The drug SCH 23390 (0.1–5 mg/kg i.p.) produced much smaller increases in 3-MT which were probably mediated through the striatonigral pathway. Overall, the data suggest that measurement of 3-MT, after inhibition of monoamine oxidase, is a useful index of the release and utilization of dopamine. However, after substantial and prolonged depletion of dopamine, levels of 3-MT in naive animals are a better index. Also, the formation of 3-MT in naive rats provides a sensitive method for distinguishing between dopamine releasing agents and reuptake inhibitors.     

强化婴幼儿奶粉中叶酸的测定

强化叶酸的奶粉在0.05M K_2HPO_4缓冲液中,经均质,调pH4.5,15000g离心20分钟,其清液调pH4.0,进行CGS树脂离子交换层析,用10ml KClK_2HPO_4洗脱,调pH7.0,进行HPLC测定,采用300x3.9mm ODS反相柱,移动相0.05M K_2HPO+MeOH(91+9),流速1ml/分,紫外检测器波长285nm,灵敏度0.0050D。方法相对标准偏差为±3.3％,回收率为87％,最小检测量为0.02μg/ml。