电感耦合等离子体质谱法测定左氧氟沙星片中8种元素杂质的含量

目的:建立电感耦合等离子体质谱(ICP-MS)法测定左氧氟沙星片中钒(V)、铁(Fe)、钴(Co)、镍(Ni)、砷(As)、镉(Cd)、汞(Hg)、铅(Pb)8种元素杂质的含量.方法:取左氧氟沙星片剂研磨成粉,用微波消解法进行处理.采用ICP-MS法进行方法学验证及样品检测,测定模式为He模式,等离子体模式为通用模式,...     

HPLC法在泊沙康唑及其15种异构体杂质拆分中的应用

建立了可同时测定泊沙康唑中15种异构体(14个立体异构体和1个位置异构体)杂质的HPLC法.采用Chiral MD(2)-RH色谱柱(4.6mmx250mm,5 μm),流动相为水:乙腈∶二乙胺(48 ∶ 52 ∶ 0.1),流速为0.6 ml/min,柱温为30℃,检测波长为260 nm.结果显示,14个立体异构体以...     

基因毒性杂质甲磺酸酯稳定性及水解反应动力学研究

目的:在痕量水平基因毒性杂质甲磺酸酯(甲磺酸甲酯、甲磺酸乙酯、甲磺酸丙酯和甲磺酸异丙酯)的稳定性及水解动力学研究.方法:以乙腈-水(80∶20,v/v)为溶剂配制甲磺酸酯混合溶液,分别置于298、313及323 K温度下,定时取样并加入碘化钠衍生化溶液,分别得到相应的碘代烷烃(碘甲烷、碘乙烷、碘丙烷和碘代异丙烷),采用...     

那格列奈及其片剂中L-异构体的HPLC测定

建立了HPLC法测定那格列奈及其片剂中的杂质L-异构体的含量.采用以α-酸性糖蛋白键合硅胶为固定相的手性色谱柱,0.02mol/L磷酸钾缓冲液(pH 7.1)-乙腈(98:2)为流动相,检测波长210nm,L-异构体检测限为2ng,平均回收率为98.0%.     

奥氮平原料药中相关杂质的合成及结构鉴定

目的合成奥氮平原料药中的相关杂质并进行结构鉴定。方法分别以奥氮平的合成中间体4-氨基-2-甲基-10H-噻吩并[2,3-b][1,5]苯二氮杂艹卓盐酸盐和奥氮平为起始原料合成奥氮平的3个相关杂质:2-甲基-10H-噻吩并[2,3-b][1,5]苯二氮杂艹卓-4-(5H)-酮(1)、1-氯甲基-1-甲基-4-(2-甲基-10H-苯并[b]噻吩并[2,3-e][1,4]二氮杂艹卓-4-哌嗪基)-1-氯化物(2)和2-甲基-4-(4-甲基-1-哌嗪基)-10H-苯并[b]噻吩并[2,3-e][1,4]二氮杂艹卓4’-N-氧化物(3)。结果与结论合成并鉴定了奥氮平质量标准中提及的3种杂质,其结构经1H-NMR、13C-NMR谱及高分辨质谱确证;并且探讨了3种杂质可能的产生途径,以期为奥氮平的质量研究和相关杂质的控制提供帮助。     

氢化可的松及其注射液有关物质检查

目的:对氢化可的松原料及其注射液中含有的有关物质进行测定。方法:采用高效液相色谱法进行分析,同时采用二极管阵列检测器进行杂质波谱扫描,液质联用法辅助确定主要杂质的结构。结果:氢化可的松和杂质峰分离良好,试验样品主要杂质确证为6,17,21β-三羟基孕甾-4-烯-3,20-二酮、表氢化可的松、17,21-二羟基孕甾-4-烯-3,20-二酮、可的松及泼尼松龙。结论:本法准确、灵敏,杂质检出性强,适用于氢化可的松及其注射液有关物质的测定。     

凝胶色谱法测定头孢拉定胶囊中的高分子杂质

目的:建立测定头孢拉定胶囊中的高分子杂质(头孢拉定聚合物)的方法。方法:采用凝胶色谱法。色谱柱为Sephadex G-10(40~120μm)凝胶柱,流动相A为0.2 mol.L-1磷酸盐缓冲液(pH 8.0),流动相B为水,流速为1.0 ml.min-1;检测波长为254 nm。结果:头孢拉定胶囊的高分子杂质含量均小于0.5%。结论:方法灵敏、准确、简便,可用于本品的质量控制,对提高临床有效性及安全性有利。以此方法测定国内10个厂家头孢拉定胶囊的高分子杂质,结果发现,香港澳美制药厂的产品高分子杂质含量最低,优于其它厂家。     

Tetrandrine and related bis—benzylisoquinoline alkaloids from medicinal herbs：cardiovascular effects and mechanisms of action

Tetrandrine(TET),a bis-benzylisoquinoline alkaloid purified and identified an active ingredient in a Chinese medicinal herb,Radix Stephanae tetrandrae,has been used traditionally for the treatment of congestive circulatory disorder and inflammatory diseases.TET,together with a few of its structural analogues,has long been demonstrated to have antihypertensive action in clinical as well as animal studies.Presumably,the primary anti-hypertensive action of TET is due to its vasodilatory properties.TET prevents or inhibits vascular contraction induced by membrane depolarization with KCl or α-adrenoceptor activation with phenylephrine (PE).TET(30μmol/L) also inhibits the release of endothelium-derived nitric oxide(NO) as well as NO production by inducible NO synthase.TET apparently inhibits multiple Ca^2 entry pathways as demonstrated in cell types lacking the L-type Ca^2 channels.In cardiac muscle cells,TET inhibits both L-and T-type Ca^2 channels.In addition to its actions on cardiovascular tissues,TET may also exert its anti-hypertensive action via a Ca^2 -dependent manner on other tissues intimately involved in the modulation of blood pressure control,such as adrenal grands.In adrenal glomerulosa cells,KCl-or angiotensin II-induced aldosterone synthesis is highly dependent on extracellular Ca^2 .Steroidogenesis and Ca^2 -influx in bovine adrenal glomerulosa cells have been shown to be potently inhibited by TET.In bovine adrenal chromaffin cells,TET inhibits Ca^2 currents via L-and N-type channels as well as other unidentified channels with IC50 of 10μmol/L.Other than the Ca^2 antagonistic effects.TET also interacts with the α-adrenergic receptors and muscarinic receptors based on functional as well as radioligand binding studies.Apart from its functional effects,TET and related compounds also exert effects on tissue structures,such as remodelling of hypertrophied heart and inhibition of angiogenesis,probably by causing apoptotic responses.TET is also known for its anti-inflammatory and anti-fibrogenic actions,which make TET and related compound potentially useful in the treatment of lung silicosis,liver cirrhosis,and rheumatoid arthritis.     

盐酸普拉克索降解杂质BI-IO460BS的合成

报道了盐酸普拉克索降解杂质BI-IO460BS的合成方法.焦谷氨醇经对甲苯磺酰氯取代、氰化钾氰化、碘丙烷N-丙基化、氰解并甲酯化、氧硫交换、氨腈取代、水解得BI-IO460BS.反应总收率为5.9％,并经MS和1H NMR等进行了结构确证.     

ICP-AES法同时测定碳酸锂原料药中6种杂质元素

目的：建立电感耦合等离子体发射光谱（ICP-AES)同时测定碳酸锂原料药中6种杂质元素（钙、钠、钾、镁、铁和铝）的分析方法,并分析不同厂商碳酸锂原料药的杂质含量。方法：用硝酸溶解样品, ICP-AES法分析样品中6种杂质元素的含量。结果：6种元素标准曲线的相关系数均高于0.999,加标回收率为93%～99%,检出限为0.0003～0.1275μg·mL-1,RSD值均小于2%;利用本法对5个厂家使用的碳酸锂原料药进行测定,结果表明C厂的原料药中钙、钠、镁、铁和铝元素含量均高于其余4个厂家,其中钠超出了药典规定限度。结论：与《中国药典》中碳酸锂原料药杂质测定方法进行比对,本试验所建立的方法测定结果与药典方法一致,且方法专属性强、灵敏度高、操作简单,可以用于碳酸锂原料药中6种杂质元素的测定。