On-line Raman spectroscopy of ribonucleotides preconcentrated by capillary isotachophoresis.
On-line Raman spectroscopy of ribonucleotides preconcentrated by capillary isotachophoresis.
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通过毛细管等速电泳预浓缩核糖核苷酸的在线拉曼光谱。
DOI：
10.1021/ac00119a009
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发表时间：
1995
影响因子：
7.4
通讯作者：
Morris,MD
中科院分区：
文献类型：
--
作者：
Walker3rd,PA;Kowalchyk,WK;Morris,MD
常规拉曼光谱用作磷酸盐缓冲液中腺苷5 '-三磷酸、腺苷5'-二磷酸和腺苷5 '-单磷酸的毛细管等速电泳（ITP）的在线检测器。预浓缩是从1 × 10-2 M磷酸盐缓冲液（pH 7.5）到0.1 MKCl或Na 2SO 4的前导电解质中，终止电解质为0.1 M 4-吗啉丙烷琥珀酸。核糖核苷酸在检测窗口处被浓缩到10 ~（-2）M以上，允许从5 × 10~（-2）M或更高的起始浓度测量具有1 s积分的拉曼光谱。表示“高”之义在一个固有的简单和快速的实验1中的分辨率分离被缺乏广泛适用的检测方法所平衡，质量信息。最流行的检测方法，紫外吸收，2激光诱导荧光，3和电化学，4只提供有关分离的定量信息。洗脱分析物的阳性鉴定通常需要对样品有广泛的先验知识，并与适当的迁移率标准品进行比较。软电离技术，电喷雾质谱（MS）5和快原子轰击MS，6已成功地连接到CE。这些提供分子量信息，但具有很少或没有碎片化。已经有成功的低频质子核磁共振谱（1H NMR）在电泳毛细管中的有前途的报告。7毛细管共振、预共振和正常拉曼
Normal Raman spectroscopy is used as an on-line detector for capillaryisotachophoresis (ITP) of adenosine 5'-triphosphate, adenosine 5'-diphosphate, and adenosine 5'-monophosphate in phosphate buffers. Preconcentra-tion is from a 1 x 10-2 M phosphate buffer (pH 7.5) into a leading electrolyte of 0.1 Mkc1 or Na2SC> 4, with a terminating electrolyte of 0.1 M 4-morpholinepropanesutfonic acid. The ribonucleotides are concentrated to above 10-2M at the detection window, allowing measure-ment of Raman spectra with 1 s integration, from starting concentrations of 5 x 10~* 123456 M or higher.The familiar capillary electrophoresis (CE) advantages of rapid, high-resolution separations in an inherently simple and rapid experiment1 are balanced by the lack of widely applicable detection methods with a high content of qualitative information. The most popular detection methods, UV absorbance, 2 laser-induced fluo-rescence, 3 and electrochemistry, 4offer only quantitative information about the separation. Positive identification of the eluted analytes usually requires extensive prior knowledge of the sample and comparison to appropriate mobility standards. The soft ionization techniques, electrospray mass spectrometry (MS) 5 and fast atom bombardment MS, 6 have been successfully interfaced to CE. These provide molecular weight information, but with little or no fragmentation. There have been promising reports of successful low-frequency proton nuclear magnetic resonance spectroscopy (H NMR) in electrophoresis capillaries. 7 On-capillary resonance, preresonance, and normal Raman