摘要
本文建立了一种固相萃取-气相色谱-质谱检测法,用于检测水产加工制品中5种酚类抗氧化剂残留。5种酚类抗氧化剂为二丁基羟基甲苯（BHT）、丁基羟基茴香醚（BHA）、特丁基对苯二酚（TBHQ）、4-己基间苯二酚（4-HR）和没食子酸丙酯（PG）。研究过程如下：用乙酸乙酯提取样品,硅胶柱净化,正己烷、乙酸乙酯洗脱,气相色谱-质谱测定,外标法定量。研究显示：在质量浓度为0.05-10μg/mL范围内,抗氧化剂的响应值与质量浓度的线性关系良好,相关系数为0.997 1-0.999 8。在0.05-1mg/kg添加浓度下,丁香鱼干、虾干和干贝加标样品的日内和日间平均回收率为70.6%-119%,相对标准偏差为1.09-9.80%;BHT、BHA、TBHQ和4-HR的检出限为0.01mg/kg,最低定量限为0.05mg/kg;PG的检出限为0.05mg/kg,最低定量限为0.25mg/kg。研究结果表明,本文建立的固相萃取-气相色谱-质谱检测法可以有效的检测出水产加工制品中的5种酚类抗氧化剂残留。
Antioxidant is a kind of food additive, which can prevent food ingredients due to oxidation and lead to deterioration. It is mainly used to preventing oxidative rancidity of fats and fat rich food, as well as oxidation caused by fading browning and destruction of vitamin among others. The research on the detec- tion method of antioxidants has been widely carried out in the oil, feed, fried food and convenience food, but the research on the animal source food is scarce. Research on the detection method of phenolic antioxi- dants in aquatic products is still blank. Gas chromatography-mass spectrometry （GC-MS） coupled with solid-phase extraction was developed for determining five phenol antioxidants residue in processed aquatic products including butylated hydroxyl anisole （BHA）, tert-butylhydroquinone （TBHQ）, butylated hy- droxyl toluene （BHT）, propyl gallate （PG） and 4-hexylresorcinol （4-HR）. The effects of different extrac- ting agents, extraction times, solid-phase extraction columns, elution solutions and elution volume on the extraction were investigated. The phenol antioxidants were extracted with ethyl acetate, purified by silica gel column and eluted with n-hexane and ethyl acetate, then quantified with GC-MS by referring to the ex- ternal standards. With the optimized method, recovery tests were done by adding antioxidant mixed stan- dard solution at different concentrations to dried anchovy, shrimp and scallop blank samples of intra-day and inter-day. The linear range was 0. 05-10 /μg/mL and the correlation coefficient was 0. 997 1-0. 999 8. When spiked within 0.05-1 mg/kg, the average recovery of intra-day and inter-day was 70. 6G-119G, and the relative standard deviation was 1.09%-9.80%. The limit of detection and quantitation of BHT, BHA, TBHQ and 4-HR was 0.01 mg/kg and 0.05 mg/kg, respectively. The limit of detection and quanti- tation of PG was 0.05 mg/kg and 0. 25 mg/kg, respectively. This method is simple; the sample has a short detection period, the reagent dosage is litt
出处
《中国海洋大学学报（自然科学版）》
CAS
CSCD
北大核心
2016年第8期64-71,共8页
Periodical of Ocean University of China
基金
福建省省属公益类科研院所基本科研专项(2013R001-6)
福建省海洋高新产业发展专项(闽海洋高新[2014]18号)资助~~
关键词
酚类抗氧化剂
气相色谱-质谱法
水产加工制品
残留
phenol antioxidant
chromatography-mass spectrometryl processed aquatic products
residue
