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新型表面聚合型手性固定相的制备及应用

Preparation and application of the novel chiral stationary phase by surface-initiated polymerization
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摘要 采用(S)-2-氨甲基四氢吡咯作为手性单体,以键合在3-氨丙基硅胶上的4,4'-偶氮-二(4-氰基)戊酸(ACVA)作为引发剂,通过直接引发表面聚合反应,制备了一种新型HPLC刷型手性固定相CSP-a。采用乙腈-甲醇为流动相,在柱温30℃和UV 254 nm检测条件下实现了对联萘酚衍生物、氨基酸衍生物的色谱拆分。结果表明,CSP-a对π酸和π碱类化合物都有明显拆分效果。 A novel brush-type chiral stationary phase(CSP-a) for HPLC were prepared by surfaced-initiated polymerization with(S)-2-aminomethylpyrrolidine as a chiral monomer and dichloride of 4,4′-azo-bis-4-cyanopentanoic acid bonded on the surface of silica gel as a radical initiator.The resolutions of the enantiomers of binaphthol derivatives and amino acid derivatives on CSP-a were carried out using acetonitrile/methanol as mobile phases under the detection conditions of column temperature of 30 ℃ and UV wavelength of 254 nm.The results indicate that CSP-a was effective for the resolutions of the enantiomers of π-acid and π-base derivatives.
出处 《化学试剂》 CAS CSCD 北大核心 2013年第4期356-358,共3页 Chemical Reagents
基金 西安文理学院院级重大课题资助项目(zd2009-04)
关键词 手性固定相 (S)-2-氨甲基四氢吡咯 对映体拆分 联萘酚衍生物 氨基酸衍生物 chiral stationary phase (S)-2-aminomethylpyrrolidine enantioseparation binaphthol derivatives amino acid derivatives
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参考文献3

  • 1DIAKOS C I, ZHANG M, BEALE P J, et al. Synthesis, charaeterisation and in vitro eytotoxieity studies of a series of chiral platinum (Ⅱ) complexes based on the 2-aminomethylpyrrolidine ligand: X-ray crystal structure of [ PtCl2 (R-dimepyrr)] ( R-dimepyrr = N-dimethyl- 2 (R) -aminomethylpyrrolidine) [ J ]. Eur. J. Med. Chem. , 2009,44(7) :2 807-2 814.
  • 2BEESLOY T E,TRAHANOVSKY W S, ARMSTRONG D W,et al. Chromatographic evaluation of poly (trans-1,2- cyclohexanediyl-bisacrylamide ) as a chiral stationary phase for HPLC [ J ]. J. Chromatogr. A, 2005,1 066 ( 1 ) : 55-70.
  • 3GASPARRINI F, MISITI D, ROMPIETTI R, et al. New hybrid polymeric liquid chromatography chiral stationary phase prepared by surface-initiated polymerization [ J ]. J. Chromatogr. A,2005,1 064 ( 1 ) : 25-38.

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