海产品中溴酚类海洋风味素的气相色谱-质谱联用分析  

Analysis of bromophenol-like marine flavors in marine aquatic products by gas chromatography-mass spectrometry

作　　者：徐继林[1] 严小军[1] 徐年军[1] 沈佳[1] 沈丽君[1] 

机构地区：[1]宁波大学海洋生物工程重点实验室,浙江宁波315211

出　　处：《水产学报》2004年第1期100-105,共6页Journal of Fisheries of China

基　　金：国家新药基金(2003AA2Z3511);浙江省青年人才基金(RC02059)

摘　　要：建立了海产品中的溴酚类海洋风味素的毛细管气相色谱-质谱联用检测法。样品中溴酚类化合物在挥发油测定器中用乙酸乙酯通过循环蒸馏萃取,浓缩后用电子轰击源在特征离子碎片扫描检测模式下进行检测。结果表明,5种溴酚类化合物在SBP-50柱上得到良好的分离,色谱出峰尖锐,没有杂峰干扰。本方法在2.5～40 mg·L^(-1)浓度范围内线性关系良好,最低检测限低于1ng·mL^(-1)。当向25.00g样品中添加溴苯酚各2.0μg时,平均回收率分别达到90.45％(2-BP)、60.49％(4-BP)、85.79％(2,4-DBP)、84.98％(2,6-DBP)、90.80％(2,4,6-TBP),标准相对偏差为1.37％～4.16％。对市场上销售的几种海洋经济动物测定,溴酚类风味素含量在5.40～31.38 ng·g^(-1)范围内,而所测得的淡水青虾中溴酚类风味素含量只有0.18 ng·g^(-1)。A sensitive analytical method of bromophenol-like marine flavors has been established using capillary gas chromatography-mass spectrometry. The bromophenols in the aquatic products can be extracted by essential oil analyzer effectively, and determined using EI - SIM - MS after concentration. The results indicated that five bromophenol compounds can be separated from each other on SBP - 50 column, with sharp peak and rare contamination. The linearity is superior from 2.5 to 40 mg·L^(-1), with low detection limit of 1 ng·mL^(-1). The average recovery rate is 90.45% for 2 - BP, 60.49% for 4 - BP, 85.79% for 2,4 - DBP, 84.98% for 2,6 -DBP, and 90.80 % for 2,4,6 - TBP, respectively, after spiking each bromophenol 2.0μg into 25.00 g sample. The standard deviation ranges from 1.37 to 4.16%. This method is applied to determine the bromophenol compounds in different aquatic products, with the results of 5.40-31.38 ng·g^(-1) for seafoods including two species of shrimp, one species of clam, and one species of fish, and only 0.18 ng·g^(-1) for fresh seafood (freshwater shrimp).

关 键 词：海产品 溴酚类海洋风味素 气相色谱-质谱联用 含量测定 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]