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有机氟键合相高效液体色谱填料的研究 Ⅰ.全氟酰胺键合堆积硅珠的制备及其在甾族化合物分析中的应用

STUDIES ON THE FLUORO-ORGANIC BONDED PHASE AS HPLC PACKING I. PREPARATION OF PERFLUORO-AMIDE BONDED AGGREGATED SILICA AND ITS APPLICATION IN STEROID ANALYSIS

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【作者】 李文华王锦华陈立佛胡振元

【Author】 LI WEN-HUA WANG JIN-HUA CHEN LI-FO HU ZHEN-YUAN (Shanghai Institute of Organic Chemistry, Academia Sinica)

【机构】 中国科学院上海有机化学研究所中国科学院上海有机化学研究所

【摘要】 我们将Υ-(全氟辛酰胺基)丙基三乙氧基硅烷,CF3(CF26CONH(CH2)Si(OC2H53,与堆积硅珠(比表面积300m2/g)键合,使其表面改性.根据元素分析计算出此填料上的有机层复盖量为5%,键合基为Υ-(全氟辛酰胺基)丙基一乙氧基硅烷,表面层浓度0.3μmol/m2.它的色谱极性较硅胶小,对多羟基甾体及共轭烯酮类化合物有较好的分离作用.曾应用于筋骨草激素、蜕皮激素、孕甾烯酮、螺旋内酯、副肾皮质酮、黄体酮及其它甾族化合物的分析分离.

【Abstract】 Treatment of aggregated silica beads with γ-(perfluorocapryl amido)-propyl riethyloxysilane, CF3(CF26CONH(CH23Si(OC2H53, gave rise to a new perfluoroamide bonded PLC packing that was oalled F-N bonded packing. From its carbon and fluorine content, it is believed that he ligand group has a γ- (perfluorocapryl amido)-propyl monoethoxy structure and its coverage is around %. The specific surface area of the aggregated silica beads is 300 m2/g, so the surface concentration of his ligand group is about 0.3μmol/m2. This F-N bonded packing is much less polar than its parent aterial, and shows good selectivities towards compounds containing different numbers of conjugated ouble ond and hydroxyl groups. This packing is good for the separation of 5β-hydroxy-β-ecdyson (6) and β-odysone (5), spirolactone (7) and △1-dehydrospirolactone (8), pregnenediones (1) and (2), orticosterone (11), deoxycorticosterone (10) and progesterone (9) as well as stachysterone D 3) and ajugasterone D (4).

  • 【文献出处】 化学学报 ,Acta Chimica Sinica , 编辑部邮箱 ,1981年Z1期
  • 【被引频次】4
  • 【下载频次】50
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