摘要
建立了高效液相色谱同时定量测定食品中叔丁基对羟基茴香醚、2,6-二叔丁基对甲酚、特丁基对苯二酚、没食子酸丙酯、没食子酸辛酯、没食子酸异戊酯和没食子酸月桂酯7种抗氧化剂的分析方法。液态油脂样品经甲醇反复提取后氮气吹干,5 mL甲醇定容;固体样品使用正己烷提取,再用乙腈反萃取多次,氮气吹干,5 mL甲醇定容。提取液经Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm)分离,以1.5%乙酸-甲醇为流动相,梯度洗脱。用二极管阵列检测器(PDA)进行检测,结合保留时间和紫外光谱进行定性分析,定量检测波长280 nm。7种抗氧化剂在1～100 mg/L范围内具有较好的线性关系,相关系数r2>0.999,定量下限(LOQ,S/N=10)为1.0～1.5 mg/kg;空白样品的加标回收率为79%～101%,相对标准偏差均低于7%。将该方法应用于食品中抗氧化剂的检测,从成品植物油、坚果等食品中检出抗氧化剂的残留。该方法准确快速、灵敏度高,满足食品中添加剂的检测要求。
A method was developed for the simultaneous determination of ？ antioxidants, including butylated hydroxyanisole （ BHA）, butylated hydroxytoluene （ BHT）, tertiary butylhydroquinone （ TBHQ）, propyl gallate （PG）, octyl gallate （OG）, iso-amyl gallate （IAG） and dodecyl gallate （ DG）, in food using high performance liquid chromatographic （HPLC） method. The liquid oil sample was extracted with methanol. The extract was dried under N2 and redissolved with methanol. The solid sample was extracted with hexane, and then back extracted by acetonitrile repeatedly. The extract was also dried under N2 and redissolved with methanol. The separation of analytes was performed on an Eclipse XDB -C18 column（250 mm x4. 6 mm i. d. , 5 μm） by gradient elution using methanol - 1.5% acetic acid water solution as mobile phase at a flow rate of 1. 0 mL/min. The sample was separated and detected with photodiode array detector（PDA）. The qualification analysis was performed by using retention time and UV spectrum, and the quantification analysis was based on the detection wavelength of 280 nm. Good linearities between concentrations of 7 analytes and peak area were achieved over the range of 1 - 100 mg/L with correlation coefficients（r2） larger than 0. 999. The limits of quantitation（ LOQs, S/N = 10） of 7 analytes ranged from 1.0 mg/kg to 1.5 mg/kg. The recoveries ranged from 79% to 101% , with relative standard deviations（RSDs） less than 7%. The method was successfully applied in the determination of 7 antioxidants residues in foods, such as cooking oil and nuts. The method is accurate, rapid and sensitive, and complys with the regulations for the determination of additives residues in foods.
出处
《分析测试学报》
CAS
CSCD
北大核心
2012年第10期1319-1324,共6页
Journal of Instrumental Analysis
关键词
高效液相色谱
抗氧化剂
食品
high performance liquid chromatography（HPLC）
antioxidants
food
