中空纤维膜液相微萃取技术/气相色谱-质谱法对食品中防腐剂与抗氧化剂的测定  

Determination of Preservatives and Antioxidants in Foods by Gas Chromatography-Mass Spectrometry Combined with Hollow-fibre Membrane Liquid-phase Microextraction

作　　者：向俊[1] 漆爱明[1] 毛丽秋[1] 

机构地区：[1]湖南师范大学化学生物学与中药分析省部共建教育部重点实验室,湖南长沙410081

出　　处：《分析测试学报》2009年第5期560-563,共4页Journal of Instrumental Analysis

摘　　要：将中空纤维膜液相微萃取技术与气相色谱-离子阱质谱联用,测定食品中的4种防腐剂(对羟基苯甲酸甲酯(MP)、对羟基苯甲酸乙酯(EP)、对羟基苯甲酸丙酯(PP)及对羟基苯甲酸丁酯(BP))和3种抗氧化剂(叔丁基-4-羟基苯甲醚(BHA)、叔丁基苯二酸(TBHQ)、2,6-二叔丁基对甲酚(BHT))。优化的萃取条件:以15%(质量分数)Na2SO4的盐溶液为稀释溶剂,5μL甲苯为萃取溶剂,搅拌速率为1200r/min,萃取时间为15min。该方法的线性范围为0.4～80mg/kg,检出限为0.002～8.0μg/kg,加标回收率为94%～115%,相对标准偏差为4.38%～9.34%。A method for the determination of 4 preservatives （methyl-p-hydroxybenzoate, ethyl-p- hydroxybenzoate, propyl-p-hydroxybenzoate, butyl-p-hydroxybenzoate） and 3 antioxidants （ butylated hydroxy anisol, tert-butylhydroquinone, 2, 6-di-tert-butyl-4-methylphenol） in food was developed by gas chromatography - ion trap mass spectrometry （ GC - IT/MS） combined with hollow-fibre membrane liquid-phase microextraction（HF-LPME）. The optimal extraction conditions were as follows： 15% Na2SO4 sah solution as diluent, 5.0 IxL toluene as extraction solvent, 1 200 r/min of stirring rate and 15 min of extraction time. Results showed that the linear range for the method was 0. 4 - 80 mg/ kg, the detection limits （LOD） were between 0. 002 and 8.0 μg/kg. The spiked recoveries were 94%- 115% with relative standard deviations of 4.38%- 9.34%.

关 键 词：中空纤维膜液相微萃取 气相色谱-离子阱质谱 防腐剂 抗氧化剂 食品 

分 类 号：O657.63[理学—分析化学] S482.294[理学—化学]