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以R-联萘酚为原料,利用铃木反应改进合成了已有文献报道的R-(3,3’-二苯基-1,1’-二萘基)-20-冠-6,并将其涂敷于C18硅胶(平均粒径5μm,孔径120)上制成了可用于高效液相色谱手性拆分的R-(3,3’-二苯基-1,1’-二萘基)-20-冠-6冠醚固定相(CSP).在以p H=2的高氯酸溶液为流动相,流速为0.1 m L·min-1,柱温为25℃的条件下,研究了R-(3,3’-二苯基-1,1’-二萘基)-20-冠-6冠醚固定相(CSP)对13种α-氨基酸对映体的拆分能力,并将其拆分结果与商品CR(+)柱进行了对比.实验结果表明在此色谱条件下,有11种α-氨基酸对映体(苯甘氨酸、对羟基苯甘氨酸、蛋氨酸、酪氨酸、色氨酸、缬氨酸、亮氨酸、异亮氨酸、苯丙氨酸、谷氨酸、天冬氨酸)能得到不同程度的拆分,并且对其中6种α-氨基酸对映体的拆分效果要好于商品CR(+)柱.研究表明此冠醚手性固定相对α-氨基酸对映体有很好的手性识别能力,在对α-氨基酸对映体的拆分上能与商品CR(+)柱相媲美.
R- (3,3’-diphenyl-1,1’-dinaphthyl) -20-crown-6 has been synthesized from R-binaphthol by Suzuki reaction. It was coated on C18 silica gel (average particle diameter 5μm, pore size 120) to prepare R- (3,3’-diphenyl-1,1’-dinaphthalene which can be used for chiral resolution of high performance liquid chromatography (CSP) .Under the condition of a mobile phase with p H = 2 perchloric acid as mobile phase and a flow rate of 0.1 m L · min-1 and a column temperature of 25 ℃, The resolution ability of 13 α-amino acid enantiomers of R- (3,3’-diphenyl-1,1’-dinaphthyl) -20 crown-6 crown ether stationary phase (CSP) The results were compared with the commercial CR (+) column.The experimental results show that there are 11 kinds of α-amino acid enantiomers (phenylglycine, p-hydroxyphenylglycine, methionine, tyrosine, Tryptophan, valine, leucine, isoleucine, phenylalanine, glutamic acid and aspartic acid) were isolated to some extent, and six kinds of α-amino acid enantiomers The results showed that this crown ether chiral stationary phase has good chiral recognition ability to α-amino acid enantiomer, For the resolution of enantiomers can commodity CR (+) column comparable.