Florisil固相萃取-HPLC-FLD法测定烤肉中15种多环芳烃
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摘要
建立一种Florisil固相萃取-HPLC-FLD法同时测定烤肉中15种多环芳烃(PAHs)的方法。样品经超声提取,Florisil固相萃取柱净化,通过高效液相色谱分离,外标法定量。结果表明, 15种PAHs的质量浓度在1～50 ng/mL范围内与色谱峰面积呈良好线性关系,线性相关系数(r)大于0.999 5;在5, 10和20μg/kg的加标水平下,平均回收率分别为73.1%～87.5%, 78.2%～93.3%和85.3～97.5%,相对标准偏差为2.0%～5.0%, 1.8%～5.0%和1.1%～3.1%;检出限(S/N=3)与定量限(S/N=10)分别为0.33～3.3μg/kg和1.0～10μg/kg。
A method for simultaneous determination of 15 kinds of polycyclic aromatic hydrocarbons(PAHs) in barbecue by Florisil SPE-HPLC-FLD was developed. The sample was extracted by ultrasonic extraction, purified by Florisil SPE,separated by HPLC, and quantified by external standard method. The results showed that the concentration of 15 kinds of PAHs was linear with chromatographic peak area in the range of 1-50 ng/mL. The linear correlation coefficients(r) were more than 0.999 5. At the spiking level of 5, 10 and 20 μg/kg, the average recovery was from 73.1% to 87.5%, from 78.2% to 93.3%and from 85.3% to 97.5%, and the relative standard deviation was from 2.0% to 5.0%, from 1.8% to 5.0% and from 1.1% to3.1%. The detection limits(S/N=3) were from 0.33 to 3.3 μg/kg and the quantitative limits(S/N=10) were from 1.0 to 10 μg/kg.
A method for simultaneous determination of 15 kinds of polycyclic aromatic hydrocarbons(PAHs) in barbecue by Florisil SPE-HPLC-FLD was developed. The sample was extracted by ultrasonic extraction, purified by Florisil SPE,separated by HPLC, and quantified by external standard method. The results showed that the concentration of 15 kinds of PAHs was linear with chromatographic peak area in the range of 1-50 ng/mL. The linear correlation coefficients(r) were more than 0.999 5. At the spiking level of 5, 10 and 20 μg/kg, the average recovery was from 73.1% to 87.5%, from 78.2% to 93.3%and from 85.3% to 97.5%, and the relative standard deviation was from 2.0% to 5.0%, from 1.8% to 5.0% and from 1.1% to3.1%. The detection limits(S/N=3) were from 0.33 to 3.3 μg/kg and the quantitative limits(S/N=10) were from 1.0 to 10 μg/kg.
引文
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[6]康翠欣,宋雅东,朱静璇,等. HPLC和GC-MS/MS测定食用油中4种多环芳烃的方法比较[J].食品科技, 2018, 43(3):294-299.
[7]宋晓娟,李海燕,尹明明,等.快速溶剂萃取-气相色谱-串联质谱法分析海洋沉积物中16种多环芳烃[J].色谱, 2018,36(1):51-58.
[8]彭驰,廖晓兰,王美娥,等.自动索氏-固相相萃取-GC/MS测定土壤中多环芳烃方法的建立[J].湖南农业科学,2009(6):57-60.
[9]贾敬香,潘铁英,杜一平,等.超声波萃取-GC/MS法测定橡胶轮胎中的多环芳烃[J].环境污染与防治, 2008, 30(3):54-61.
[2] STOFYHWO A, SIKORSKI Z E. Polycyclic aromatichydrocarbons in smoked fish—A critical review[J]. Food Chemistry, 2005, 91(2):303-311.
[3]罗世榕.高效液相色谱荧光法测定土壤中16种多环芳烃[J].福建分析测试, 2010, 19(2):69-72.
[4]张志玮,朱琳,刘华良,等.供体受体复合色谱法测定植物油中16种欧盟优控多环芳烃[J].中国油脂, 2012, 37(3):74-77.
[5]吕爱娟,时磊,蔡小虎,等. QuEChERS-高效液相色谱法快速测定稻谷和土壤中16种多环芳烃[J].理化检验, 2016,52(9):1017-1021.
[6]康翠欣,宋雅东,朱静璇,等. HPLC和GC-MS/MS测定食用油中4种多环芳烃的方法比较[J].食品科技, 2018, 43(3):294-299.
[7]宋晓娟,李海燕,尹明明,等.快速溶剂萃取-气相色谱-串联质谱法分析海洋沉积物中16种多环芳烃[J].色谱, 2018,36(1):51-58.
[8]彭驰,廖晓兰,王美娥,等.自动索氏-固相相萃取-GC/MS测定土壤中多环芳烃方法的建立[J].湖南农业科学,2009(6):57-60.
[9]贾敬香,潘铁英,杜一平,等.超声波萃取-GC/MS法测定橡胶轮胎中的多环芳烃[J].环境污染与防治, 2008, 30(3):54-61.