磁分散萃取结合气质谱联用法同时测定植物油中24种多环芳烃
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摘要
目的建立一种快速、高效、准确的测定植物油中24种多环芳烃(PAHs)的磁分散固相萃取-气相色谱质谱联用法。方法以自制的氨基功能化磁性碳纳米管(EDA-@Mag-CNTs)为吸附剂,经磁分散固相萃取进行富集,经甲苯洗脱后采用DB-EUPA毛细管柱和质谱检测器对植物油中多环芳烃进行检测,同位素内标法定量。结果 24种多环芳烃在1μg/L～250μg/L有很好的相关性,相关系数均> 0. 998 5,该方法最低检出限为0. 1μg/kg～1. 0μg/kg,最低定量限为0. 3μg/kg～3. 0μg/kg;在低、高2种加标水平下,回收率分别为83. 2%～96. 6%和85. 2%～98. 9%。结论本方法操作简便、快速、灵敏度高,可用于植物油中24种多环芳烃的检测。通过对27份植物油样品的测定,初步得到衢州市售植物油中多环芳烃的污染特征,通过植物油摄入多环芳烃的健康风险需引起关注。
Objective To develop a rapid,effective and accurate method for the determination of 24 polycyclic aromatic hydrocarbons( PAHs) in vegetable oils by magnetic dispersive solid-phase extraction combined with gas chromatography and mass spectrometry( MSPE-GC/MS). Methods The target PAHs were enriched,ethylenediamine-functionalized magnetic carbon nanotubes( EDA-@ Mag-CNTs),by magnetic dispersion solid phase extraction,and eluted with toluene; the polycyclic aromatic hydrocarbons in vegetable oil were detected by DB-EUPA capillary column and mass spectrometer,and quantified by isotope internal standard method. Results The 24 kinds of PAHs showed good linearity in the range of 1 μg/L-250 μg/L( r > 0. 998 5). The limits of detection( LODs) in vegetable oils of 24 PAHs were witin 0. 1 μg/kg-1. 0 μg/kg and the limits of quantification( LOQs) were within 0. 3 μg/kg-3. 0 μg/kg. Recoveries were within 83. 2%-96. 6% at low spiked level,and 85. 2%-98. 9% at high spiked level. Conclusion The developed method is simple,rapid and sensitive,and can be applied to the analysis of 24 PAHs in vegetable oils. The pollution characteristics in vegetable oil in Quzhou was preliminarily acquired by the determination of 27 samples. So,the health risks by PAHs intake from vegetable oil should be concerned.
Objective To develop a rapid,effective and accurate method for the determination of 24 polycyclic aromatic hydrocarbons( PAHs) in vegetable oils by magnetic dispersive solid-phase extraction combined with gas chromatography and mass spectrometry( MSPE-GC/MS). Methods The target PAHs were enriched,ethylenediamine-functionalized magnetic carbon nanotubes( EDA-@ Mag-CNTs),by magnetic dispersion solid phase extraction,and eluted with toluene; the polycyclic aromatic hydrocarbons in vegetable oil were detected by DB-EUPA capillary column and mass spectrometer,and quantified by isotope internal standard method. Results The 24 kinds of PAHs showed good linearity in the range of 1 μg/L-250 μg/L( r > 0. 998 5). The limits of detection( LODs) in vegetable oils of 24 PAHs were witin 0. 1 μg/kg-1. 0 μg/kg and the limits of quantification( LOQs) were within 0. 3 μg/kg-3. 0 μg/kg. Recoveries were within 83. 2%-96. 6% at low spiked level,and 85. 2%-98. 9% at high spiked level. Conclusion The developed method is simple,rapid and sensitive,and can be applied to the analysis of 24 PAHs in vegetable oils. The pollution characteristics in vegetable oil in Quzhou was preliminarily acquired by the determination of 27 samples. So,the health risks by PAHs intake from vegetable oil should be concerned.
引文
[1] Thneeya C,Akira T,Takayuki K,et al. Simultaneous determination of urinary hydroxylated metabolites of naphthalene,fluorene,phenanthrene fluoranthene and pyrene as multiple biomarkers of esposure to polycyclic aromatic hydrocarbons[J]. Anal Bioanal Chem,2006,386(3):712-718.
[2] Chen Y,Zhang J,Ma Q,et al. Human health risk assessment and source diagnosis of polycyclic aromatic hydrocarbons(PAHs)in the corn and agricultural soils along main roadside in Changchun,China[J]. Hum Ecol Risk Assess,2015,22(3):706-720.
[3] Ibanez R,Agudo A,Berenguer A,et al. Dietary intake of polycyclic aromatic hydrocarbon in a Spanish population[J]. J Food Protect,2005,68(10):2190-2195.
[4] Windal I,Boxus L,Hanot V,Validation of the analysis of the 15+1 European-priority polycyclic aromatic hydrocarbons by donnoracceptor complex chromatography and high-performance liquid chromatography-ultraviolet/fluorescence detection[J]. J Chromatogr,2008,1212(1/2):16-22.
[5]林侃.超高效液相色谱法测定大气细颗粒物中16种多环芳烃[J].中国卫生检验杂志,2017,27(17):2465-2469,2853.
[6]石飞云,靳艺,唐宏兵,等.高效液相色谱-二极管阵列检测器串联荧光检测法同时测定空气中的16种多环芳烃[J].中国卫生检验杂志,2017,27(22):3212-3214.
[7] Mottier P,Parisod V,Turesky RJ. Quantitative determination of polycyclic aromatic hydrocarbons in barbecued meat sausages by gas chromatography coupled to mass spectrometry[J]. Agric Food Chem,2000,48(4):1160-1166.
[8] Jung SY,Park JS,Chang MS,et al. A simple method for the determination of polycyclic aromatic hydrocarbons(PAH)in edible oil employing solid phase extraction(SPE)cartridge purification[J].Food Sci Biotechnol,2013,22(1):241-248.
[9]曾莉,张炤,刘丹,等.气相色谱-质谱法同时测定肉制品中的12种多环芳烃[J].中国卫生检验杂志,2017,27(17):2486-2488,2504.
[10]张永涛,张莉,李义,等.基质固相分散-稳定同位素稀释-气相色谱-质谱联用测定土壤中多环芳烃[J].中国卫生检验杂志,2017,27(7):923-925,930.
[11] Khalili-Fard V,Ghanemi K,Nikpour Y,et al. Application of sulfur microparticles for solid-phase extraction of polycyclic aromatic hydrocarbons from sea water and wastewater samples[J]. Anal Chim Acta,2012,714(3):89-97.
[12] Wang DW,Zhao SM,Jin W,et al. Simultaneous determination of28 polychlorinated biphenyls and 16 polycyclic aromatic hydrocarbons in sediments using ASE-SPE-GC-Qq Q-MS/MS[J].Chinese J Anal Chem,2013,41(6):861-868.
[13] Wang JH,Guo C,Pang GF,et al. Determination of polycyclic aromatic hydrocarbons in vegetable oils by GPC purification isotope dilution internal standard quantitative GC-MS[J]. J Instrum Anal,2009,28(3):267-271.
[14]陈东洋,张昊,冯家力,等.沉积物中15种多环芳烃的凝胶渗透色谱-高效液相色谱法[J].中国卫生检验杂志,2017,27(20):2896-2899.
[15]zhan G,zden S,Alpertunga B. Determination of commonly used herbicides in surface water using solid-phase extraction and dualcolumn HPLC-DAD[J]. J Environ Sci Heal B,2005,40(6):827-840.
[16]张蕴,吴香伦,汪尤刚,等.磁分散固相萃取-气相色谱法测定水中8种氨基甲酸酯类农药[J].中国卫生检验杂志,2016,26(11):1521-1523.
[2] Chen Y,Zhang J,Ma Q,et al. Human health risk assessment and source diagnosis of polycyclic aromatic hydrocarbons(PAHs)in the corn and agricultural soils along main roadside in Changchun,China[J]. Hum Ecol Risk Assess,2015,22(3):706-720.
[3] Ibanez R,Agudo A,Berenguer A,et al. Dietary intake of polycyclic aromatic hydrocarbon in a Spanish population[J]. J Food Protect,2005,68(10):2190-2195.
[4] Windal I,Boxus L,Hanot V,Validation of the analysis of the 15+1 European-priority polycyclic aromatic hydrocarbons by donnoracceptor complex chromatography and high-performance liquid chromatography-ultraviolet/fluorescence detection[J]. J Chromatogr,2008,1212(1/2):16-22.
[5]林侃.超高效液相色谱法测定大气细颗粒物中16种多环芳烃[J].中国卫生检验杂志,2017,27(17):2465-2469,2853.
[6]石飞云,靳艺,唐宏兵,等.高效液相色谱-二极管阵列检测器串联荧光检测法同时测定空气中的16种多环芳烃[J].中国卫生检验杂志,2017,27(22):3212-3214.
[7] Mottier P,Parisod V,Turesky RJ. Quantitative determination of polycyclic aromatic hydrocarbons in barbecued meat sausages by gas chromatography coupled to mass spectrometry[J]. Agric Food Chem,2000,48(4):1160-1166.
[8] Jung SY,Park JS,Chang MS,et al. A simple method for the determination of polycyclic aromatic hydrocarbons(PAH)in edible oil employing solid phase extraction(SPE)cartridge purification[J].Food Sci Biotechnol,2013,22(1):241-248.
[9]曾莉,张炤,刘丹,等.气相色谱-质谱法同时测定肉制品中的12种多环芳烃[J].中国卫生检验杂志,2017,27(17):2486-2488,2504.
[10]张永涛,张莉,李义,等.基质固相分散-稳定同位素稀释-气相色谱-质谱联用测定土壤中多环芳烃[J].中国卫生检验杂志,2017,27(7):923-925,930.
[11] Khalili-Fard V,Ghanemi K,Nikpour Y,et al. Application of sulfur microparticles for solid-phase extraction of polycyclic aromatic hydrocarbons from sea water and wastewater samples[J]. Anal Chim Acta,2012,714(3):89-97.
[12] Wang DW,Zhao SM,Jin W,et al. Simultaneous determination of28 polychlorinated biphenyls and 16 polycyclic aromatic hydrocarbons in sediments using ASE-SPE-GC-Qq Q-MS/MS[J].Chinese J Anal Chem,2013,41(6):861-868.
[13] Wang JH,Guo C,Pang GF,et al. Determination of polycyclic aromatic hydrocarbons in vegetable oils by GPC purification isotope dilution internal standard quantitative GC-MS[J]. J Instrum Anal,2009,28(3):267-271.
[14]陈东洋,张昊,冯家力,等.沉积物中15种多环芳烃的凝胶渗透色谱-高效液相色谱法[J].中国卫生检验杂志,2017,27(20):2896-2899.
[15]zhan G,zden S,Alpertunga B. Determination of commonly used herbicides in surface water using solid-phase extraction and dualcolumn HPLC-DAD[J]. J Environ Sci Heal B,2005,40(6):827-840.
[16]张蕴,吴香伦,汪尤刚,等.磁分散固相萃取-气相色谱法测定水中8种氨基甲酸酯类农药[J].中国卫生检验杂志,2016,26(11):1521-1523.