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.
出处
《上海海洋大学学报》
CAS
CSCD
北大核心
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)
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
subcritical water extraction
gel permeation chromatography（GPC）
gas chromatography-mass spectrometry（GC-MS）
B（a） P
smoked fish
