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JPC – Journal of Planar Chromatography – Modern TLC - Thin-layer chromatography (TLC) of fifteen amino acids was performed using silica gel and alumina impregnated with micellar... 相似文献
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《Analytical letters》2012,45(12):1285-1291
Abstract The polynuclear aromatic compounds (PNA): anthracene, napthalene, phenanthrene, pyrene, pyrenecarboxaldehyde, benzo (a) pyrene, benzo (e) pyrene, perylene and fluorene can be chromatographed on polyamide TLC sheets using an aqueous micellar solution cf sodium dodecylsulfate (SDS) as the mobile phase. Reversed micellar solutions (of sodium dioctylsulfosuccinate) were used in a reverse phase chromatographic separation of amino acids. Some amino acids tended to streak slightly rather than move as discrete spots. Conditions could be adjusted, however, so that most of the amino acids and all PNA's would move as spots. 相似文献
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计算机辅助柱色谱最优化分离氨基酸王琴孙,颜炳文,王寿亭,陶雪(南开大学元素有机化学研究所,天津,300071)(南开大学高分子化学研究所)关键词计算机,色谱最优化,柱色谱微型计算机的发展推动了整个色谱优化领域的发展,也陆续出现了一些优化分离方法[1~... 相似文献
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《液相色谱法及相关技术杂志》2012,35(16):3497-3528
Abstract Proteins are among the most important components of all living systems. Their function range from catalysts 9enzymes) to regulators to structural components. The building blocks and language of proteins are about 20 amino acids (H2N CHR COOH), linked together By peptide bonds ([sbnd]CO[sbnd]NH[sbnd]) in chains that may consist of a few dozen to more than 1000 amino acides. The determination of primary structure of proteins, namely the sequence (arrangement) of the various amino acids along the chain is still a challenging tast. Edman reaction lies virtually at the core of all modern sequencing strategies [1,2]. The N-terminal polypeptide is first coupled to phenyl isothiocyanate to from the phenylthio carbamyl peptide; this derivative is then cleaved with anhydrous acid to expose a new N-terminus and to release the original N-terminal amino acid as a 5′thiazolinone (Scheme-1). The excess reagents and by products are extracted by an organic solvent wash. The extract of thiazolinone amino acid (obtained either from liquid-phase or solid-phase degration) is evaporated and converted to the phenylhtiohydantion derivative by 5 n HCL/CH3COOH (1:2 v/v) at 52°C for 50 min. The sample is extracted with ethyl acetate, dried and redissolved in a suitable volume of ethanol for TLC identification. Repetition of this process with identification of the released PTH-amino acidsfro the N-terminal end. For smaller peptides PITC may be used to remove the amino terminal amino acid while a chromphore or fluorophore such as dansyl chloride or DABITC, which react with the newly exposed amino terminus, is used to identify the new amino terminus. Both manual and automated methodologies are currently used for small and large polypeptides which rely upon identification of amino terminal amino acid as PTH derivative. A large number of papers have been and continue to be publihsed on the analysis of the PTH derivatives of amino acides. 相似文献
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《液相色谱法及相关技术杂志》2012,35(1):161-174
Abstract An extensive study of the HPLC separation of 20 free amino acids by the addition of alkanesulfonate salts to the mobile phase was previously reported (1). This paper describes modifications in the procedure that improves the separation and resolution of the 20 free amino acids. Mobile phase variables (type and concentration of alkanesulfonate salt, organic modifier concentration, mobile phase pH, and mobile phase ionic strength), and stationary phase variables (particle size, type of packing) which can affect amino acid separation, resolution and selectivity were studied. Two stationary phases were compared, the 5 μm Hamilton PRP-1 and Phase Separations 3 μm, ODS-2. Longer chain alkanesulfonate salts (octane and decanesulfonate salts) were evaluated as mobile phase additives. A mobile phase gradient of increasing per cent organic modifier was necessary for separating complex mixtures of polar and nonpolar-basic amino acids. It is now possible to separate 19 of 20 free amino acids with this ion-interaction chromatographic procedure. 相似文献
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《液相色谱法及相关技术杂志》2012,35(7):1359-1365
Abstract Copper sulphate and polyamide were tried as impregnants for improving the separation of twenty amino acids on silica gel ‘G’ layers using a new solvent system MeOH-BuOAc-AcOH-Pyridine(20:20:10:5). Tables are presented to illustrate the improvement in resolution of amino acids on silica gel plates. 相似文献
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JPC – Journal of Planar Chromatography – Modern TLC - 相似文献
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《液相色谱法及相关技术杂志》2012,35(15):3049-3065
Abstract It has been detected that racemization of amino acids in metabolically stable proteins of living mammals takes place (1–4) and as a consequence the protein-structure function relationship may be altered (5). Thus in vitro and in vivo analysis of racemic amino acids is very important. Besides enantiomeric purity becomes very significant when only one of the enantiomers has a potential biological activity for example L-DOPA (3,4-dihydroxypheny 1 alanine) is an important drug for treating Parkingson's disease. The measurement of specific rotation is a common and well accepted method for evaluating hydrophile-hydrophile interactions between the second carboxyl group of amino acid and the alkaline substructures of adenine (probably hydrogen-bond formation); hydrophobe-hydrophobe interactions between the apolar sidechain of the amino acid and the corresponding adenine substructures. 相似文献
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毛细管电动色谱带电环糊精拆分N—FMOC氨基酸对映体 总被引:3,自引:0,他引:3
将负电性磺丁基-β-环糊精手性添加剂应用于毛细管电泳氨基酸对映体的拆分研究中,对8种氨基酸对映体与9-芴甲基氧基甲酰氯(FMOC-Cl)生成的衍生物进行了分离,其中5种得到了基线分离。考察了背景电解质pH值及磺丁基-β-环糊精的浓度对N-FMOC氨基酸对映体拆分的影响。 相似文献
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用芯片毛细管电泳激光诱导荧光检测系统研究了分离多种荧光素异硫氰酸酯(FITC)衍生氨基酸的实验条件.采用以乙醇为有机添加剂的胶束毛细管电动色谱分离体系(50 mmol/LSDS,体积分数为15%的乙醇,5 mmol/L pH 9.2的硼砂缓冲液),在72 mm长的通道上实现了10种常见氨基酸的分离,一次分离的时间小于5 min. 相似文献
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Four neutral amino acids (Gly, Ala,.Val and Leu) were separated with ligand exchange resins. The separation capacity of the ligand exchange resins is compared with that of common ion exchange resins. The effects of eluent, column temperature, and central metal ions of the support on the separation are studied. The relationship between matrix structure of resins and their separation capacity is analysed. 相似文献
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Sajewicz Mieczysław Piętka Robert Drabik Gabriela Namysło Ewa Kowalska Teresa 《平面色谱法杂志一现代薄层色谱法》2006,19(4):273-277
JPC – Journal of Planar Chromatography – Modern TLC - We have previously discussed in detail thin-layer chromatographic studies of the retention of the 2-arylpropionic acids (2-APA)... 相似文献
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对一种分离测定氨基酸方法的改进 总被引:17,自引:4,他引:17
对Waters公司采用 6 氨基喹啉 N 羟基琥珀酰亚胺基 氨基甲酸酯 (AccQ Tag)柱前衍生化测定氨基酸的方法进行了改进。将流动相流速由原来的 1 0mL/min改变为 2 0mL/min ,用AccQ Tag专用柱 (3 9mmi.d .× 15 0mm ,4μm)在 17 5min(原为 35min) (运行周期为 2 2 5min ,原为 45min)内快速分离测定了 18种氨基酸和牛磺酸。用Nova PakC18柱 (3 9mmi.d .× 15 0mm ,4μm) ,Nova PakC18柱 (4 6mmi.d .× 15 0mm ,4μm) ,SymmetryC18柱 (3 9mmi.d .× 15 0mm ,4μm)和WatersXterraRP 18柱等反相C18柱代替AccQ Tag专用柱 ,均可对氨基酸进行快速分离。 相似文献
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《Analytical letters》2012,45(7):1429-1437
Abstract Enantiomers of alanine, methionine, tryptophan, serine, threonine, phenylalanine, tyrosine, and glutamic acid are sampled respectively in different channel of a new capillary array electrophoresis with rotary fluorescence scanner that was built by ourselves and separation conditions for these respective enantiomers are screened with different types and concentrations of additives to the separation buffer. The experimental results indicate that 2.5 mM β‐cyclodextrin additives are preferred for the respective separation of the eight kinds of amino acids. 相似文献
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制药废液中氨基酸的分离与测定 总被引:1,自引:0,他引:1
为测定维生素 B12 制药厂排出的废液中氨基酸量,先在所取的废液样品中加入乙酸铅使其中蛋白质及其他大分子有机物产生沉淀并用离心法分离.上层澄清液中的氨基酸通过装有强酸性阳离子交换树脂的交换柱(25 cm×2.5 cm)予以分离,用1 mol·L-1 氨水将氨基酸从柱上洗脱.在所得洗脱液中用气相色谱-质谱及傅立叶变换红外光谱法对氨基酸进行定性及定量测定. 相似文献