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
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上海海洋大学 食品学院,上海出入境检验检疫局 动植物与食品检验检疫技术中心,上海出入境检验检疫局 动植物与食品检验检疫技术中心,上海出入境检验检疫局 动植物与食品检验检疫技术中心,上海海洋大学 食品学院;上海出入境检验检疫局 动植物与食品检验检疫技术中心,上海出入境检验检疫局 动植物与食品检验检疫技术中心,上海出入境检验检疫局 动植物与食品检验检疫技术中心

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


Determination of benzo(a)pyrene residue in smoked fish by subcritical water extraction and gas chromatography-mass spectrometry
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College of food,Shanghai Ocean University,Technical Center of Inspection Quarantine in plants、animals and food,Shanghai Entry-Exit Inspection and Quarantine Bureau,Technical Center of Inspection Quarantine in plants、animals and food,Shanghai Entry-Exit Inspection and Quarantine Bureau,Technical Center of Inspection Quarantine in plants、animals and food,Shanghai Entry-Exit Inspection and Quarantine Bureau,College of food,Shanghai Ocean University;China;Technical Center of Inspection Quarantine in plants、animals and food,Shanghai Entry-Exit Inspection and Quarantine Bureau;China,Technical Center of Inspection Quarantine in plants、animals and food,Shanghai Entry-Exit Inspection and Quarantine Bureau,Technical Center of Inspection Quarantine in plants、animals and food,Shanghai Entry-Exit Inspection and Quarantine Bureau

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    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。

    Abstract:

    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/mL 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 of 2.5, 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.

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史思,伊雄海,赵善贞,邓晓军,陈舜胜,樊祥,朱坚.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[J].上海海洋大学学报,2014,23(6):948-953.
SHI Si, YI Xiong-hai, ZHAO Shan-zhen, DENG Xiao-jun, CHEN Shun-sheng, FAN Xiang, ZHU Jian. Determination of benzo(a)pyrene residue in smoked fish by subcritical water extraction and gas chromatography-mass spectrometry[J]. Journal of Shanghai Ocean University,2014,23(6):948-953.

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  • 收稿日期:2014-04-18
  • 最后修改日期:2014-06-16
  • 录用日期:2014-08-25
  • 在线发布日期: 2014-11-21
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