亚临界水萃取及气相色谱-质谱法测定烟熏鱼中苯并(a)芘残留  

Determination of benzo( a ) pyrene residue in smoked fish by subcritical water extraction and gas chromatography-mass spectrometry

作　　者：史思[1] 伊雄海[2] 赵善贞[2] 邓晓军[2] 陈舜胜[1] 樊祥[2] 朱坚[2] 

机构地区：[1]上海海洋大学食品学院,上海201306 [2]上海出入境检验检疫局动植物与食品检验检疫技术中心,上海200135

出　　处：《上海海洋大学学报》2014年第6期948-953,共6页Journal of Shanghai Ocean University

基　　金：质检公益行业科研专项(201010073-04);质检公益行业科研专项(201110019-04)

摘　　要：建立了亚临界水萃取（SCWE）及气相色谱-质谱（GC-MS）检测熏鱼中苯并（a）芘残留的方法。实验表明,样品经100℃的亚临界水提取5 min后,将目标物转移至环己烷-乙酸乙酯（1∶1,V/V）中,经凝胶渗透色谱（GPC）净化,Rtx-5MS毛细管气相色谱柱分离,在选择离子监测（SIM）模式下检测。目标物在0~100 ng/mL范围内线性关系良好,相关系数大于0.9999,其定量限为2.5 ng/g,检出限为1 ng/g。烟熏鱼基质中添加2.5、5和10 ng/g三个水平的标准品时,苯并（a）芘的回收率为74.89%~114.01%,相对标准偏差（RSD）为7.95%~10.56%（n=8）。该方法的灵敏度良好、准确度和精密度均符合分析要求,适用于烟熏鱼中苯并（a）芘残留的检测。A method was developed for the B（ a） P determination in smoked fish by gas chromatography-mass spectrometry（ GC-MS） method with subcritical water extraction（ SCWE）. B（ a） P were extracted by water under the extraction temperature of 100 ℃ for 5 min,transferred into cyclohexane-ethylacetate（ 1 ∶ 1,V / V）and then cleaned up by the Gel Permeation Chromatography（ GPC）. The GC separation was performed on a Rtx-5MS capillary column. The B（ a） P were determined by MS in selected ion monitoring（ SIM） mode. The method showed good linearity over the range of 0 to 100 ng / m L with the correlation coefficient of 0. 9999. The limit of quantification（ S / N 10） was 2. 5 ng / g,the limit of detection（ S / N 10） was 1 ng / g and the precision（ RSD） was between 7. 95% and 10. 56%. The average blank spike recoveries at three levels of2. 5,5 and 10 ng / g ranged from 74. 89% to 114. 01%（ n = 8）. The sensitivity,accuracy and precision of the method are suitable for the determination of the B（ a） P in smoked fish.

关 键 词：亚临界水萃取 凝胶渗透色谱 气相色谱-质谱 苯并(A)芘 烟熏鱼 

分 类 号：TS207.7[轻工技术与工程—食品科学]