用制备型高效液相色谱分离石油亚砜的馏分

Separation of Petroleum Sulfoxides by Preparative High Performance Liquid Chromatography

用经典硅胶柱色谱法对石油亚砜 (PSO)进行预分离。PSO被分成 4个馏分 (分别记为PSO1,PSO2 ,PSO3和PSO4)。所用的流动相及洗脱顺序 :苯、二氯甲烷、甲醇 二氯甲烷 (1∶1体积比 )、甲醇。经预分离后 ,PSO中的亚砜成分主要富集在馏分PSO3和PSO2中。用高效制备液相色谱法对这两馏分作进一步的分离和纯化。PSO2的色谱条件是 :色谱柱 μ BondapakC1 85 7mm× 30 0mm ;流动相为二氯甲烷、环己烷、甲醇混合液 ,收集经纯化后的组分PSO2g2 2 ;PSO3被分离为 7个馏分 ,其色谱条件为 :色谱柱μ BondapakC1 85 7mm× 30 0mm ;流动相为 70 %～ 10 0 %甲醇 水 ;梯度洗脱其流量为 80mL min ;进样量为80mL 次 (PSO3用 70 %甲醇 水稀释 10倍 )。取其中较纯的馏分PSO3c ,PSO3e ,PSO3g作进一步的色谱纯化 ,色谱条件为C1 8半制备色谱柱 7.8mm× 30 0mm ;流速 :2 0mL min ;流动相 :甲醇 水 70∶ 30 ,V/V(PSO3c)″80∶2 0 ,V V(PSO3e) ;85∶15 ,V V(PSO3g) ;检测器UV 2 5

Petroleum sulfoxides (PSO), obtained from petroleum by-produces, were prepared by pretreatment with conventional silica gel column chromatography. The eluents applied in sequence were benzene, dichloromethane, 1 : 1 dichloromethane-methanol and methanol. In this way, PSO was separated into four fractions. The sulfoxide in PSO was largely concentrated in the second and the third fraction, namely PSO2 and PSO3, which comprised stronger polar compounds. Then PSO2 was further separated and purified by preparative high performance liquid chromatography (prep-HPLC). Its purified fraction was named PSO2g22. PSO3 was further separated into seven fractions by prep-HPLC. The conditions were as follow: mu Bondapak C-18 preparative column, 57 x 300 mm; flow rate, 80 mL/min; a mixture of methanol-water as mobile phase, gradient elution; sample size 80 mL/time; detection wavelength UV-254 nm. The three fractions of them, PSO3c, PSO3e and PSO3g, which contained high content sulfinyl sulphur, were purified by semi-preparative column, mu Bondapak C-18, 7.8 x 300 mm, and 70% and 80% aqueous solution of methanol as mobile phase for PSO3c and PSO3e, and CH3OH-H(2)0 85: 15 (V/V) and 100% methanol for PSO3g respectively.