大孔树脂-磁场辅助溶剂结晶联合纯化红松籽油甾醇的研究  

Purification of Sterols from Korean Pine Seed Oil by Macroporous Resin Combined with Magnetic Field Assisted Solvent Crystallization

作　　者：王莉莉 包怡红[1] 赵庆佳 张娜[2] 郭庆启[1,3] Wang Lili;Bao Yihong;Zhao Qingjia;Zhang Na;Guo Qingqi(School of Forestry,Northeast Forestry University,Haerbin 150040;College of Food Engineering,Harbin University of Commerce,Haerbin 150028;Key Laboratory of Forest Food Resources Utilization of Heilongjiang Province,Haerbin 150040)

机构地区：[1]东北林业大学林学院,哈尔滨150040 [2]哈尔滨商业大学食品工程学院,哈尔滨150028 [3]黑龙江省森林食品资源利用重点实验室,哈尔滨150040

出　　处：《中国粮油学报》2022年第8期222-230,共9页Journal of the Chinese Cereals and Oils Association

基　　金：中央高校基本科研业务费专项资金(2572018BA09);黑龙江省自然科学基金(ZD2019C002)。

摘　　要：采用大孔树脂对红松籽油甾醇进行初步纯化,再利用磁场辅助溶剂结晶对其进行二次纯化。通过对比5种大孔树脂对红松籽油甾醇的吸附及解吸效果,筛选出AB-8树脂为最佳纯化介质,其纯化红松籽油甾醇的最佳工艺条件为:上样质量浓度0.2 mg/mL,上样量30 mL,吸附流速2 mL/min,吸附时间3 h,解吸液乙醇体积分数80%,乙醇体积70 mL,解吸流速2 mL/min,解吸时间4 h,此工艺条件下红松籽油甾醇纯度为(45.32±2.13)%。磁场辅助溶剂结晶纯化红松籽油甾醇的最佳工艺参数为:磁场强度0.3 T,以无水乙醇为结晶溶剂,料液比1∶10,养晶温度5℃,养晶时间4 h,此工艺条件下红松籽油甾醇纯度为(83.12±3.24)%。纯化后的红松籽油甾醇经光谱扫描,210 nm处出现植物甾醇的特征峰带,经红外光谱扫描分析,具有植物甾醇类物质的特征吸收峰,经气相色谱-质谱鉴定出2种植物甾醇,分别为β-谷甾醇和菜油甾醇,且β-谷甾醇占红松籽油甾醇总量的80%以上。The macroporous resin was used to preliminarily purify the sterols of Korean pine seeds,and the magnetic field assisted solvent crystallization was used to purify it for the second time.By comparing the adsorption and desorption effects of five macroporous resins on Korean pine seed oil sterol,AB-8 resin was selected as the best purification medium.The optimal process conditions for purifying Korean pine seed oil sterol were as follows:loading mass concentration of 0.2 mg/mL,loading volume of 30 mL,adsorption flow rate of 2 mL/min,adsorption time of 3 h,ethanol volume fraction of desorption solution of 80%,ethanol volume of 70 mL,desorption flow rate of 2 mL/min,the desorption time of 4 h.Under these conditions,the purity of sterol in Korean pine seed oil was(45.32±2.13)%.The optimum technological parameters for purification of Korean pine seed oil sterol by magnetic field assisted solvent crystallization were as follows:magnetic field intensity of 0.3 T,with the anhydrous ethanol as crystallization solvent,solid-liquid ratio of 1∶10,crystallization temperature of 5℃,crystallization time of 4 h.Under these technological conditions,the purity of Korean pine seed oil sterol was(83.12±3.24)%.After spectral scanning,the characteristic peak of purified sterol appeared at 210 nm;it had the characteristic absorption peak of phytosterol after infrared spectrum scanning analysis.Two kinds of phytosterols(β-sitosterol and campesterol)were identified by gas chromatography-mass spectrometry,andβ-sitosterol account for more than 80%of the total amount of Korean pine seed oil sterol.

关 键 词：大孔树脂 磁场辅助溶剂结晶 红松籽油甾醇 纯化 

分 类 号：Q946.48[生物学—植物学]