Alkylated and silylated β-cyclodextrin for gas chromatographic chiral stationary phases

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Silylated and acetylated β-cyclodextrins for gas chromatographic stationary phases

Ｓｅｐａｒａｔｉｏｎｏｆｅｎａｎｔｉｏｍｅｒｓｏｆｃｈｉｒａｌｃｏｍ ｐｏｕｎｄｓｆｏｒｂｏｔｈａｎａｌｙｔｉｃａｌａｎｄｐｒｅｐａｒａｔｉｖｅｐｕｒｐｏｓｅｓｉｓａｎａｔｔｒａｃｔｉｖｅｔｏｐｉｃ ,ｅｓｐｅｃｉａｌｌｙｉｎｔｈｅｆｉｅｌｄｓｏｆｏｒ ｇａｎｉｃａｎｄｐｈａｒｍａｃｅｕｔｉｃａｌｃｈｅｍｉｓｔｒｙ .Ｄｉｒｅｃｔｇａｓｃｈｒｏｍａｔｏｇｒａｐｈｉｃｅｎａｎｔｉｏｍｅｒｓｅｐａｒａｔｉｏｎｕｓｉｎｇｃｈｉｒａｌｓｔａｔｉｏｎａｒｙｐｈａｓｅｓ (ＣＳＰｓ)ｉｓａｓｉｍｐｌｅａｎｄｅｆｆｅ…     

Silylated and acetylated β-cyclodextrins for gas chromatographic stationary phases

Two new chiral stationary phases, 2,3-di-O-acetyl-6-O-trimethylsilyl-β-cyclodextrin (DATBCD) and 2, 6-di-O-trimethylsilyl-3-O-acetyl-β-cyclodextrin (DTABCD), were synthesized, their structures were identified by means of infrared and NMR spectra. Capillary columns were coated with the two stationary phases by dynamic method. The chromatographic properties, and enantiomers separation, such as ketone, esters, alcohols and olefines, were investigated on the silylated and acetylated β-cyclodextrin stationary phases. The experimental results show that the silylated and acetylated β-cyclodextrins are suitable to be used as capillary gas chromatographic stationary phases, the relative polarity of DATBCD and DTABCD stationary phases is respectively 4143 and 3928, the column efficiencies are respectively 3084 and 4198, and DATBCD is of stronger enantioselectivity than DTABCD, capacity factor of the first eluted enantiomer (k ₁) and separation factor(α)of α-phenylethanol on DATBCD stationary phase are respectively 8.23 and 1.019. Biography of first author: TANG Ke-wen, doctoral student, born in 1970, majoring in applied chemistry.     

Selectivity of New β-Cyclodextrin Derivatives as CGC Stationary Phases and Application for the Analysis of Volatile Compounds in Traditional Chinese Medicines

New cyclodextrin derivatives(CDs),heptakis(2,6-di-O-methyl-3-O-methoxymethyl)-β-CD(Ⅰ)and heptakis(2,3,6-tri-O-methoxymethyl)-β-CD(Ⅱ),were investigated for their chromatographic performance as stationary phases for capillary gas chromatography(CGC).Both of the CDs exhibited good selectivity and satisfactory separation for test mixtures and aromatic positional isomers,and volatile compounds from Ligusticum chuanxiong Hort.Additionally,the selectivity and elution orders of major compounds were compared with a ...     

新型GC固定相的制备及其对手性化合物的拆分研究

合成了纤维素三(3,5-二甲基苯基氨基甲酸酯)并用作气相色谱固定相,制备出手性毛细管柱,考察它的极性、柱效和手性选择性.研究表明,该固定相为中等极性,理论塔板数达1 895 m-1,容量因子1.52.该柱成功地分离了随机选取的25种(包括醇、醚、胺、酯、醛、酮、氨基酸类)外消旋化合物中的20种,其中以(±)-Dihydrocarvylacetate、(±)-Roseoxide、(±)-N-Benzyl-1-phenylethylamine、(±)-Fenchone、DL-Leucine、DL-Isoleucine拆分效果较好,证实该柱具有良好的手性分离性能,可用于气相色谱.     

一种新的环糊精接枝聚硅氧烷毛细管气相色谱固定相的分离性能

合成了一种新的环糊精接枝聚硅氧烷衍生物,单环(2,6-二-O-苄基-3-O-丙基(3'))-六环(2,6-二-O-苄基-3-O-甲基)-β-环糊精接枝聚硅氧烷衍生物,并考察了其毛细管气相色谱性能.结果表明其对一些二取代苯的位置异构体及一些光学异构体具有分离能力,是一种良好的毛细管气相色谱固定相.研究发现将环糊精衍生物接枝聚硅氧烷以及将未接枝的环糊精衍生物与OV-7混涂均可降低环糊精衍生物的极性.在较低的测试温度下,环糊精接枝聚硅氧烷固定相的分离能力比未接枝的环糊精衍生物及其与OV-7混涂固定相的分离能力强,而在高温下,三者的分离能力接近.氢硅烷化反应是降低环糊精衍生物使用温度的有效方法.