Gas chromatographic separation of ribonucleotides by means of trimethylsilyl (TMS) derivatives.

Gas chromatographic separation of ribonucleotides by means of trimethylsilyl (TMS) derivatives.
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利用三甲基甲硅烷基 (TMS) 衍生物对核糖核苷酸进行气相色谱分离。

DOI:
10.1016/0003-2697(66)90272-7
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发表时间:
1966
影响因子:
2.9
通讯作者:
Yukiko Sasaki
Yukiko Sasaki
中科院分区:
生物学4区
文献类型:
--
作者:
Takeshi Hashizume;Yukiko Sasaki

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直到最近,用气体clo - n -照相法分离核苷酸的可行性还没有确定。早期的工作已经证明了T的分离和定量的可能性;\IS核苷和碱基的温度编程气相色谱(1,2)。本通讯的目的是描述气相色谱分离TM8核糖核的可能性,idcs,并提出一个有用的补充现有的分离核苷酸的方法。用磷酸酐与1 ~三羧基二硅酸钠(3)和正磷酸与3 ~三羧基二硅酸钠(4)反应合成了磷酸三羧基二硅酸钠(4)。而用磷酸三异二醇或磷酸三钾与己烷~乙基二氮杂烷(HMDS)和三甲基二氮杂烷(TMCS)组成的三甲基化剂反应,能以相当的收率合成该化合物。该化合物为无色易溶液体,bp 910/ 5mmhg,气相色谱时形成对称峰。同样,bis (TAB)苯基磷酸(II),/L, ‘ ’”1.4590。11.1 ~。在相同配比下,可获得92%的产率
Until recently, the feasibility of separating nucleotides by gas clro~ n:-tography has not, been certain. Earlier work had shown the possibility of separation and quantification of the T;\IS nucleosides and bases by tcmptrature-programed gas chromatography (1, 2). The object of this communication is to describe the possibility of gas chromatographir separation of the TM8 ribonucleot, idcs, and to present, a useful addition to the existing methods of separating nucleotides. Tris (TMS) phosphate II 1 has been synthesized by the reactions between phosphoric anhydridc and l~ esanwtl~ yldisilosanc (3)) and orthophosphoric acid and trin~ ctl~ ylcl~ loroailanc (TMCS)(4). However, nc were able to synthesize this compound by reacting trisodiunl phosphtc or tripotassium phosphate with a trimethyleilylating agent consisting of hexan~ ethyldisilazane (HMDS) and TMCS in fair yield. This compound was a colorless and clist8illablc liquid of bp 910/5 mm Hg, and formed a symmetrical peak when gas chromatographed. Similarly, bis (TAB) phenylphosphate (II),/L,,‘” 1.4590. 11.1~. 133’~ 134”/4 mm, was obtained in 92% yield under the same con (lition; i men-