薄层色谱法测定氧氟沙星注射液中有关物质

薄层色谱法测定氧氟沙星注射液中有关物质宋刚王平周岩梁红于丽颖采用薄层色谱法，以蒸馏水为稀释溶剂，以硅胶Ⅱ（０．１％ＣＭＣ－Ｎａ水溶液制）为固定相，以乙酸乙酯－异丙醇－水－６Ｎ氨水（１５∶１３∶９∶２）为流动相，测定氧氟沙星注射液中有关物质，结果与现行...     

RP-HPLC法同时测定复方氧氟沙星滴鼻液中两组分的含量

ＲＰ－ＨＰＬＣ法,在ＳｈｉｍｐａｃｋＣＬＣ－ＯＤＳ柱上同时测定复方氧氟沙星滴鼻液中氧氟沙星和地塞米松磷酸钠的含量。平均回收率氧氟沙星为９９．８±０．５％,地塞米松磷酸钠为１００．６±０．８％（ｎ＝５）。     

薄层色谱法测定氧氟沙星注射液中有关物质

采用薄层色谱法，以蒸馏水为稀释溶剂，以硅胶Ｈ（０．１％ ＣＭＣ－Ｎａ水溶液制）为固定相，以乙酸乙酯－异丙醇－水－６Ｎ氨水（１５：１３：９：２为流动相，测定氧氟沙星注射液中有关物质，结果与现行部颁标准的高效液相色谱法一致．     

左氧氟沙星片剂的分光光度测定

左氧氟沙星（ｌｅｖｏｆｌｏｘａｃｉｎ,１）为口服氟喹诺酮类抗菌药,系氧氟沙星（ｏｆｌｏｘａｃｉｎ）的光学Ｓ－（－）异构体,其抗菌作用是氧氟沙星的两倍,为Ｒ－（＋）－氧氟沙星的８～１２８倍［１］。本品于１９９４年初在日本首次上市,商品名Ｃｒａｖｉｔ,适...     

β—环糊精流动相和手性配位交换HPLC法分离药物对映体

目的：为生物样品手性药物对照体的分离测定建立手性流动相添加剂ＨＰＬＣ。方法：以β－环糊精和手性配位交换剂对流动相添加剂，分离测定了生物样品中羟基苯妥英，美芬妥英，叔丁喘安，氯噻酮，氧氟沙星等５种手性药物对映体。结果：测得结果各对映体之间均能得到较好的分离。     

TLC—荧光分光光度法测定尿中氧氟沙星的排出速率

本文报道了用ＴＬＣ－荧光分光光度法测定２名健康受试者尿中氧氟沙星的排出速率。薄层板为硅胶Ｇ板，展开剂为苯－甲醇－甲酸（１．６７：５：３．３３）。尿样经薄层层析后，收集氧氟沙星的斑点，用乙酸－乙醇－水（９：３：１０）洗脱，于λｅｘ＝２９４ｎｍ、λｅｍ＝４９５ｎｍ处测定其荧光强度，在２０￣８００ｕｇ／ｍｌ浓度范围内呈线性，回归方程为Ｆ＝０．１３＋０．５５Ｃ，最低检出限为１０ｕｇ／ｍｌ。该法灵敏、重现性     

单胺菌素─喹诺酮酰胺衍生物的合成

为探索喹诺酮类化合物充当单胺菌素３位边链酸的构效关系，合成了４个未见文献报道的单胺菌素－喹诺酮酰胺衍生物（５ａ）～（５ｄ）．它们是以氧氟沙星（８）、氟罗沙星（９）或诺氟沙星前体（１－乙基－６－氟－７－氯－１，４－二氢－４－氧代喹啉－３－羧酸）（１０）通过ＤＣＣ－ＨＯＢＴ法酰化卡芦莫南母核（６）或氨曲南母核（７）得到的．初步体外抑菌试验表明：（５ａ）～（５ｄ）的最低抑菌浓度（ＭＩＣ）均大于１００ｍｇ／Ｌ     

氧氟沙星注射液的制备

氧氟沙星注射液的制备胡汉昆查仲玲但菊开（湖北医科大学附属第二医院武汉４３００７１）氧氟沙星（ｏｆｌｏｘａｃｉｎ）经试验以盐酸调节ｐＨ值进行配制，效果满意，现报道如下。１仪器与试剂仪器７５６ＭＣ型可见－紫外分光光度计（上海第三分析仪器厂）；ＰＨ５－３Ｃ...     

RP-HPLC手性流动相添加剂法分析尿中氧氟沙星对映体

以L-苯丙氨酸为配合剂,Cu²⁺为配合离子,建立了一种简便的手性配合交换RP-HPLC拆分氧氟沙星对映体的方法,该法已用于人尿中氧氟沙星对映异构体的分析。     

氧氟沙星复合膜的制备与质量控制

氧氟沙星复合膜以ＰＶＡ（－０４８６）－ＣＭＣＮａ（２：１）为成膜材料，ＰＶＡ（－０４８６）为覆盖膜材料，采用流涎法制备，用紫外分光光度法测定含量，平均加样回收率为９７．４７％，ＲＳＤ为１．６１％。     

新型手性配体的合成及其在沙美特罗关键中间体合成中的应用

目的合成沙美特罗的关键手性中间体。方法设计合成新型手性配体单磺酰化1，2-双-（3，5-二甲基苯基）乙二胺，通过与金属铑配合生成手性催化剂，利用该催化剂催化沙美特罗的关键手性中间体的不对称氢转移反应。结果与结论新型手性配体具有良好的催化活性和对映体选择性，催化合成得到的沙美特罗中间体的对映体选择性的ee％值为91％。     

手性药物对映体的环糊精手性流动相、手性固定相HPLC法拆分

使用β-环糊精(CD)作为手性流动相添加剂或手性固定相,采用反相高效液相色谱法首次拆分了抗胆碱能药物盐酸戊乙奎醚、盐酸苯环壬酯和盐酸卡马特灵。结果表明,3个手性药物4对对映体完全达到基线分离。求得其包络常数、包络比和分离度,并结合其他结构类似的化合物,从结构—分离因子关系的角度研究了其拆分机理。详细研究了影响容量因子和分离度的各种因素。     

手性流动相HPLC法拆分氟比洛芬对映体研究

目的:建立氟比洛芬手性药物的高效液相色谱拆分方法.方法:利用C18柱,以β-环糊精及其衍生物作为手性流动相添加剂,调节有机修饰剂比例和添加不同量的峰型修饰剂对氟比洛芬对映体进行拆分.结果:采用单6-L-脯氨酸-β-环糊精作为手性流动相添加剂,利用C18柱可直接拆分S,R-氟比洛芬对映体.最佳色谱分离条件为:流动相为1.4％的6 -L - proline -β - CD甲醇溶液(w/v):pH为4.0,体积分数1.0％的三乙胺水溶液(V/V) =25:75(V/V);柱温t=25℃;流速1.0ml/min;进样量10ul,检测波长254nm.S,R-氟比洛芬对映体获得了良好分离,分离度为1.65.结论:建立的手性流动相添加剂法能有效拆分氟比洛芬对映体.     

Analysis of optically active compounds using conventional chromatography with a circular dichroism detector

Analysis of optically active compounds in complex samples is often based on chiral chromatography or capillary electrophoresis in order to separate the enantiomers. This requires a chiral reagent, when using conventional chromatography, or an expensive chiral column, or a chiral selector, when using capillary electrophoresis. The type of column, reagent, or additive depends highly on the compound to be analysed. A simple and generally applicable method is using a conventional HPLC column coupled to a CD detector. Separation of enantiomers is not required, as they can be identified by a positive or negative peak. A racemate does not produce a peak; neither does an optically inactive compound. The application of HPLC-CD for the identification of pharmacologically active compounds, such as dexamphetamine, 5-hydroxytryptophan, (-)-huperzine A, and interferon, as standards, in registered drugs, in falsifications, and in food supplements is described.     

HPLC万古霉素手性柱和手性流动相添加剂法分离酮洛芬对映体

目的以万古霉素为手性选择子,建立酮洛芬对映体以手性柱法和流动相添加剂法进行手性分析的方法。方法考察万古霉素用量、有机改性剂用量及缓冲液pH值对酮洛芬对映体手性拆分的影响,并进行了定量分析的方法验证。结果两种拆分方法都使酮洛芬对映体达到了基线分离,都适合于酮洛芬对映体的定性和定量分析。结论所建立的两种方法均可用于S-(+)-酮洛芬的光学纯度检测。     

HPLC法拆分氟比洛芬对映体

建立氟比洛芬手性药物的高效液相色谱拆分方法。方法:手性流动相添加剂HPLC法:利用C18柱,以羟丙基-β-环糊精作为手性流动相添加剂,调节有机修饰剂甲醇的比例和添加不同量的三乙胺对氟比洛芬进行拆分;手性固定相HPLC法:利用Chiral-pakAD手性柱,以正己烷-乙腈为流动相基本成分,调整两者不同比例和添加不同量的三乙胺,对氟比洛芬进行拆分。结果:手性流动相添加剂法:使用C18柱对氟比洛芬对映异构体进行拆分,调节流动相中有机修饰剂甲醇浓度、手性流动相添加剂羟丙基环糊精浓度、峰型修饰剂三乙胺的浓度等都不能使氟比洛芬对映体达到基线分离,只能部分分离。手性固定相法:氟比洛芬对映体在Chiral-pakAD手性柱上能达到较好的分离。在正己烷-乙腈流动相系统中,正己烷体积含量为90%,三乙胺体积含量为0.05%的条件下,氟比洛芬对映体得到了较好的分离,分离度为10.0。结论:建立的手性固定相法能有效拆分氟比洛芬对映体而手性流动相添加剂法不能拆分氟比洛芬对映体。     

Synthesis and properties of optically active organoantimony compounds

The chemistry of chiral ligands for transition metal-catalyzed asymmetric reactions is an interesting research field in synthetic chemistry and has recently been the focus of much attention. Although a number of chiral ligands containing phosphorus (P) and arsenic (As) have been widely studied and are well documented, asymmetric reactions with optically active organoantimony compounds have not been reported so far. We are interested in the synthesis and utilization of optically active organoantimony compounds for asymmetric synthesis. We present here the synthesis and resolution of Sb-chiral and C2-symmetric compounds containing antimony as well as their physical and chemical properties. Resolution of (+/-)-1-phenyl-2-trimetylsilylstibindole (1), Sb (R/S)-(aryl) [2-(S)-(1-dimethylaminoethyl) phenyl] (p-tolyl) stibane (9), and (+/-)-2,2'-bis(diarylstibano)-1,1'-binaphthyl (13) can be achieved by the separation of a mixture of the diastereomeric antimony-palladium complexes. The optically pure Sb-chiral stibanes (1, 9) isolated here were optically stable, and no racemization on the chiral antimony center was observed even when they were heated under a neutral or a basic condition. Single-crystal X-ray analysis of Sb-chiral triarylstibane 9b-B revealed the presence of an intramolecular interaction between the antimony and nitrogen atoms. The optically active BINASb (13) can be used as powerful chiral ligand for the palladium-catalyzed asymmetric allylic alkylation of racemic 1,3-diphenyl-2-propen-1-yl acetate with dimethyl malonate. We also report the synthesis, molecular structure, and fluxional behavior of the (R)-(-)-7-p-tolyl-dinaphtho [2, 1-b; 1',2'-d] stibole (21c) which is the first isolated example of optically active C2-symmetric group 15 dinaphthoheteroles.     

Mirror images: the analysis of pharmaceutical enantiomers.

Pharmaceutical enantiomers often exhibit different pharmacodynamic and pharmacokinetic properties. Stereospecific chromatographic assays are available to separate these stereoisomers. Therapeutic agents often contain chemical functional groups (e.g. amino, hydroxyl, carbonyl, and carboxylic acid). These can be reacted with enantiomerically pure reagents to give diastereoisomers suitable for analysis on achiral gas chromatographic (GC) and high performance liquid chromatographic (HPLC) columns. Alternatively, derivatized or underivatized drugs may be resolved on chiral chromatographic phases. A wide variety of GC (e.g. amino acid, cyclodextrin, and metal-complex) and HPLC (mobile phase additive, crown ether, pi-pi interaction and related phases, protein, cyclodextrin, polysaccharide, methacrylate and amide polymer, and ligand exchange) columns are commercially available. This article reviews the chromatographic separation of enantiomers.     

Synthesis and application of novel biaryl compounds with axial chirality as catalysts in enantioselective reactions

A highly efficient process of aerobic oxidative coupling of 2-naphthol derivatives catalyzed by Cu(OH)Cl.TMEDA has been developed. Enantioselective oxidative coupling of 2-naphthol derivatives was achieved by the use of a chiral catalyst prepared from proline-derived diamine and cuprous chloride, affording the corresponding BINOL derivatives in good enantioselectivities of up to 78% ee. A new catalytic, enantioselective allylation of aldehydes with allyltrichlorosilanes exploiting (S)-3,3'-dimethyl-2,2'-biquinoline N,N'-dioxide as a catalyst affords homoallylic alcohols in virtually complete diastereoselectivities and high enantioselectivities of up to 92% ee, wherein the use of diisopropylethylamine as an additive has proven to be crucial for the acceleration of the catalytic cycle. It is also noteworthy that the above finding represents the first successful example of asymmetric reactions utilizing amine N-oxide as a chiral catalyst.