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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
引用本文:申世刚,宋炜,沙润甲,李挥,张敬轩.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[J].河北大学学报(自然科学版),2012(1):42-46,67.
作者姓名:申世刚  宋炜  沙润甲  李挥  张敬轩
作者单位: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;河北省食品质量监督检验研究院
基金项目: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.

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

Determination of phenolic antioxidants in oil and fried foods by GPC-SPE-HPLC
SHEN Shi-gang,SONG Wei,SHA Run-jia,LI Hui,ZHANG Jing-xuan.Determination of phenolic antioxidants in oil and fried foods by GPC-SPE-HPLC[J].Journal of Hebei University (Natural Science Edition),2012(1):42-46,67.
Authors:SHEN Shi-gang  SONG Wei  SHA Run-jia  LI Hui  ZHANG Jing-xuan
Institution:1.College of Chemistry and Environmental Science,Key Laboratory of Medical Chemistry and Molecular Diagnosis,Hebei University,Baoding 071002,China;2.Hebei Institute of Food Quality Supervision Inspection and Research,Shijiazhuang 050051,China)
Abstract: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.
Keywords:GPC  SPE  HPLC  phenolic antioxidants  oil and fried foods
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