School of Pharmacy, Nihon University, 7-7-1, Narashinodai, Funabashi-shi, Chiba 274-8555, Japan.
School of Pharmacy, Nihon University, 7-7-1, Narashinodai, Funabashi-shi, Chiba 274-8555, Japan.
J Chromatogr A. 2019 Jul 5;1596:134-141. doi: 10.1016/j.chroma.2019.03.010. Epub 2019 Mar 6.
The partition efficiencies of three different coiled columns, conventional multilayer coiled column, eccentric coiled column and toroidal coiled column, were evaluated by the separation of 4-methylumbelliferyl sugar derivatives using the coil satellite centrifuge (CSC) with an organic-aqueous two-phase solvent system composed of ethyl acetate/1-butanol/water. The CSC apparatus was reinforced the planet axis to maintain the stable satellite motion, which was completed by combining the rotation of three axes including the sun axis (the angular velocity, ω), the planet axis (ω) and the satellite axis (ω) under the relation at ω = ω + ω. In the present study, four different rotation speed combination types were used for the separation at the ratio (ω, ω, ω) = I. (300, 150, 150), II. (300, 100, 200), III. (300, 147, 153) and IV. (300, 200, 100 rpm) under different revolution speeds of ω = 300, 400 and 500 rpm. In the conventional multilayer coiled column with the upper mobile phase, the rotation speed combination type II yielded the best peak resolution while the rotation speed combination types III and IV had extremely low stationary phase retention even at higher revolution speeds. This inconvenience was eliminated by using the eccentric and the toroidal coiled column. The rotation speed combination type II for the eccentric coiled column and the type IV for the toroidal coiled column produced the best separation in both the upper and the lower mobile phases among four different rotation speed combination types. The overall results indicated that better peak resolution was obtained by the eccentric coiled column than by the toroidal coiled column except for the separation with the upper mobile phase at the low revolution speed.
三种不同螺旋柱,即常规多层螺旋柱、偏心螺旋柱和环形螺旋柱的分配效率,通过使用由乙酸乙酯/正丁醇/水组成的有机-水两相溶剂系统的线圈卫星离心机(CSC),对 4-甲基伞形酮糖衍生物的分离来评估。CSC 仪器加固了行星轴,以保持稳定的卫星运动,这是通过将三个轴(太阳轴、行星轴和卫星轴)的旋转组合来完成的,其角速度为ω=ω+ω。在本研究中,在分离时使用了四种不同的转速组合类型,比例为(ω,ω,ω)=I.(300,150,150)、II.(300,100,200)、III.(300,147,153)和 IV.(300,200,100 rpm),转速ω分别为 300、400 和 500 rpm。在具有上相的常规多层螺旋柱中,转速组合类型 II 产生了最佳的峰分辨率,而转速组合类型 III 和 IV 在更高的转速下甚至具有极低的固定相保留率。通过使用偏心螺旋柱和环形螺旋柱可以消除这种不便。对于偏心螺旋柱,转速组合类型 II,对于环形螺旋柱,转速组合类型 IV,在四种不同的转速组合类型中,在上相和下相都产生了最佳的分离效果。总的来说,除了在低转速下使用上相进行分离外,偏心螺旋柱比环形螺旋柱获得了更好的峰分辨率。