凝胶渗透色谱-固相萃取-高效液相色谱法测定油脂及油炸食品中的酚类抗氧化剂  

Determination of phenolic antioxidants in oil and fried foods by GPC-SPE-HPLC

作　　者：申世刚[1] 宋炜[1] 沙润甲[1] 李挥[1,2] 张敬轩 

机构地区：[1]河北大学化学与环境科学学院,教育部药物化学与分子诊断重点实验室,河北保定071002 [2]河北省食品质量监督检验研究院,河北石家庄050051

出　　处：《河北大学学报（自然科学版）》2012年第1期42-46,67,共6页Journal of Hebei University(Natural Science Edition)

基　　金：河北省平台建设与基础研究重点计划项目(09965120D)

摘　　要：建立了使用凝胶渗透色谱-固相萃取-高效液相色谱(GPC-SPE-HPLC)测定油脂及油炸食品中的4种常见酚类抗氧化剂没食子酸丙酯(PG)、叔丁基对苯二酚(TBHQ)、叔丁基对羟基茴香醚(BHA)和二丁基羟基甲苯(BHT)的方法.试样经乙酸乙酯-环己烷(V(乙酸乙酯)∶V(环已烷)=1∶1)和乙腈漩涡振荡萃取,凝胶渗透色谱(GPC)和HLB固相萃取柱净化,以乙腈-体积分数为0.1%甲酸水溶液为流动相,以BDS HYPERSIL C18柱作为分离柱,在检测波长280nm下用紫外检测器检测.方法的检出限为0.6～1.0mg/kg(油脂样品)和0.3～0.5mg/kg(油炸样品),定量限为2～3mg/kg(油脂样品)和1～1.7mg/kg(油炸样品),线性相关系数r>0.998,平均回收率为80.3%～94.0%(油脂样品)和80.3%～93.4%(油炸样品);相对标准偏差(RSD)为3.22%～8.80%(油脂样品)和2.74%～9.62%(油炸样品).该方法选择性好,灵敏度高,检出限低,能够成功地应用于油脂及油炸食品中4种常见酚类抗氧化剂的检测.A method has been developed for the determination of four phenolic antioxidants,namely propyl gallate（PG）,tertiary butylhydroquinone（TBHQ）,butylated hydroxyanisole（BHA） and butylated hydroxytoluene（BHT） in oil and fried foods by gel permeation chromatography＇solid phase extraction-high performance liquid chromatograph（GPC-SPE-HPLC）.The sample was extracted with cyclohexane/ethyl acetate mixture（1∶1,V/V） and acetonitrile on a vortex mixer,cleaned up through gel permeation chromatography and follow a further HLB solid phase extraction,eluted by the mobile phase of acetonitrile-water containing 0.1% formic acid with BDS HYPERSIL C18 column as the separation column,the eluents were determined by HPLC at wavelength of 280nm using ultraviolet detector.The limits of detection（LOD）was 0.6-1.0mg/kg（oil）and 0.30-0.50mg/kg（fried foods）,the limits of quantification（LOQ）was 2.0-3.0mg/kg（oil）and 1.0-1.7mg/kg（fried foods）,the calibration curves showed good linearity with correlation coefficients larger than 0.998,the mean recoveries were in the range of 80.3%-94.0%（oil）and 80.3%-93.4%（fried foods）,and accordingly the relative standard deviation ranged from 3.22%-8.80% （oil）and 2.74%-9.62%（fried foods）.The method is of high sensitivity,low detection limit,good determination,and can be used to accurately determine four phenolic antioxidants in oil and fried foods.

关 键 词：凝胶渗透色谱 固相萃取柱 高效液相色谱 酚类抗氧化剂 油脂及油炸食品 

分 类 号：O657.7[理学—分析化学]