2种前处理技术/气相色谱-质谱技术测定食用植物油中16种多环芳烃残留量及其对比研究
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摘要
目的比较2种前处理技术/气相色谱-质谱技术测定食用植物油中16种多环芳烃残留量。方法本研究利用QuEChERS(quick,easy,cheap,effective,ruggedandsafe)和凝胶渗透色谱(gelpermeation chromatography, GPC)2种前处理技术对样品进行处理,并采用16种多环芳烃全指标同位素内标法定量。比较使用QuEChERS和GPC 2种不同前处理方法的净化效果和方法学参数。结果 16种多环芳烃在10～200 ng/mL范围内线性关系良好,相关系数均大于0.995,定量限为0.3～0.8μg/kg。使用QuEChERS前处理方法的平均回收率和相对标准偏差(relative standard deviation, RSD)分别为88.9%～112.3%和3.6%～12.9%,使用GPC方法的平均回收率和RSD分别为86.2%～107.7%和3.0%～7.3%。对实验室内食用植物油样品进行测定, 2种方法检测结果基本一致。结论 2种前处理方法的精确度和稳定性均较好,均可用于食用植物油中16种多环芳烃残留量的测定。
Objective To compare the determination of 16 kinds of polycyclic aromatic hydrocarbons(PAHs) in edible vegetable oil by 2 kinds of pretreatment methods/gas chromatography-mass spectrometry(GC-MS). MethodsThe samples were pretreated by 2 kinds of methods including QuEChERS(quick, easy, cheap, effective, rugged and safe) and gel permeation chromatography(GPC) methods. The 16 PAHs were quantified by isotopic internal standard method. The purification effect and methodological parameters of 2 different pretreatment methods of QuEChERS and GPC were compared. Results Sixteen PAHs had good linear relationships in the range of 10-200 ng/mL with the correlation coefficients were greater than 0.995. The limits of quantitation(LOQs) were in the range of 0.3-0.8 μg/kg. The average recoveries were 88.9%-112.3% with the relative standard deviations(RSDs) of 3.6%-12.9% when QuEChERS was used as pretreatment method. The average recoveries were 86.2%-107.7% with the RSDs of 3.0%-7.3% by using GPC. The determination results of edible vegetable oil samples using 2 different pretreatments in the laboratory were basically the same. Conclusion The 2 kinds of different pretreatment methods are accurate and stable, which can be used for the determination of 16 kinds of PAHs residues in edible vegetable oil.
Objective To compare the determination of 16 kinds of polycyclic aromatic hydrocarbons(PAHs) in edible vegetable oil by 2 kinds of pretreatment methods/gas chromatography-mass spectrometry(GC-MS). MethodsThe samples were pretreated by 2 kinds of methods including QuEChERS(quick, easy, cheap, effective, rugged and safe) and gel permeation chromatography(GPC) methods. The 16 PAHs were quantified by isotopic internal standard method. The purification effect and methodological parameters of 2 different pretreatment methods of QuEChERS and GPC were compared. Results Sixteen PAHs had good linear relationships in the range of 10-200 ng/mL with the correlation coefficients were greater than 0.995. The limits of quantitation(LOQs) were in the range of 0.3-0.8 μg/kg. The average recoveries were 88.9%-112.3% with the relative standard deviations(RSDs) of 3.6%-12.9% when QuEChERS was used as pretreatment method. The average recoveries were 86.2%-107.7% with the RSDs of 3.0%-7.3% by using GPC. The determination results of edible vegetable oil samples using 2 different pretreatments in the laboratory were basically the same. Conclusion The 2 kinds of different pretreatment methods are accurate and stable, which can be used for the determination of 16 kinds of PAHs residues in edible vegetable oil.
引文
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[15]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-化学分册,2016,52(9):1017-1021.Lv AJ,Shi L,Cai XH,et al.QuEChERS-high performance liquid chromatography for rapid determination of 16 polycyclic aromatic hydrocarbons in rice and soil[J].Phys Chem Anal B,2016,52(9):1017-1021.
[16]Lucas LZD.PAH analysis in salmon with enhanced matrix removal-lipid[J].Food Test Agric Environ,2015.https://www.agilent.com/cs/library/applications/5991-6088EN.pdf
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[18]方杰,王凯雄.气相色谱-离子阱质谱法测定海洋贝类中多残留有机氯农药、多氯联苯和多环芳烃[J].分析化学,2007,35(11):1607-1613.Fang J,Wang KX.Determination of polychlorinated pesticides,polychlorinated biphenyls and polycyclic aromatic hydrocarbons in marine shellfish by gas chromatography-ion trap mass spectrometry[J].Anal Chem,2007,35(11):1607-1613.
[19]孙红梅,朱玉梅,周军.GC/MS/MS法测定土壤中16种多环芳烃的仪器条件[J].环境与发展,2017,29(7):132-134.Sun HM,Zhu YM,Zhou J.Instrumental conditions for the determination of 16 polycyclic aromatic hydrocarbons in soil by GC/MS/MS[J].Environ Dev,2017,29(7):132-134.
[20]周华,张蕴,张喆骅,等.高分子印迹固相萃取技术结合GC/MS法测定食用油中16种多环芳烃[J].卫生研究,2016,(6):957-962.Zhou H,Zhang Y,Zhang ZH,et al.Determination of 16 polycyclic aromatic hydrocarbons in edible oil by polymer imprinted solid phase extraction and GC/MS[J].J Hyg Res,2016,(6):957-962.
[21]吴性良,朱万森,马林.分析化学原理[M].北京:化学工业出版社,2010.Wu XL,Zhu WS,Ma L.Principles of analytical chemistry[M].Beijing:Chemical Industry Press,2010.
[2]张小涛,刘玉兰,王月华.食用油脂中多环芳烃的研究进展[J].中国油脂,2012,37(10):45-49.Zhang XT,Liu YL,Wang YH.Research progress of polycyclic aromatic hydrocarbons in edible oils and fats[J].China Oils Fats,2012,37(10):45-49.
[3]岳敏,谷学新,邹洪,等.多环芳烃的危害与防治[J].首都师范大学学报,2003,24(3):40-44.Yue M,Gu XX,Zou H,et al.Harm and prevention of polycyclic aromatic hydrocarbons[J].J Cap Norm univ,2003,24(3):40-44.
[4]雒建伟,高良敏,陈一佳,等.持久性有机污染物(POPs)的环境问题及其治理措施研究进展[J].环保科技,2016,22(6):51-55.Ge JW,Gao LM,Chen YJ,et al.Research progress on environmental problems and treatment measures of persistent organic pollutants(POPs)[J].Environ Prot Technol,2016,22(6):51-55.
[5]王丽,金芬,张雪莲,等.食品中多环芳烃及卤代多环芳烃的研究进展[J].食品工业科技,2012,33(10):369-373.Wang L,Jin F,Zhang XL,et al.Research progress of polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons in food[J].Sci Technol Food Ind,2012,33(10):369-373.
[6]GB/T 24893-2010动植物油脂多环芳烃的测定[S].GB/T 24893-2010 Animal and vegetable oils-Determination of polycyclic aromatic hydrocarbons[S].
[7]GB/T 23213-2008植物油中多环芳烃的测定气相色谱-质谱法[S].GB/T 23213-2008 Determination of polycyclic aromatic hydrocarbons in vegetable oils-GC-MS method[S].
[8]SN/T 1877.3-2007矿物油中多环芳烃的测定方法[S].SN/T 1877.3-2007 Determination of polycyclic aromatic hydrocarbons in mineral oil[S].
[9]SN/T 4943-2017食品级润滑油(脂)中多环芳烃的测定气相色谱-质谱联用法[S].SN/T 4943-2017 Determination of polycyclic aromatic hydrocarbons in food grade lubricating oils-GC-MS method[S].
[10]王国庆,王宗义,程明捷,等.冷冻除脂-气相色谱-串联质谱法检测食用植物油中30种多环芳烃[J].食品科学,2018,39(8):282-287.Wang GQ,Wang ZY,Cheng MJ,et al.Determination of 30 polycyclic aromatic hydrocarbons in edible vegetable oils by freeze defatting combined with gas chromatography-tandem mass spectrometry[J].Food Sci,2018,39(8):282-287.
[11]Veyrand B,Brosseaud A,Sarcher L,et al.Innovative method for determination of 19 polycyclic aromatic hydrocarbons in food and oil samples using gas chromatography coupled to tandem mass spectrometry based on an isotope dilution approach[J].J Chromatogr A,2007,1149(2):333-344.
[12]徐文君,王峰,朱晓军,等.气质联用法测定食用植物油中的多环芳烃[J].江苏农业科学,2014,42(11):339-341.Xu WJ,Wang F,Zhu XJ,et al.Determination of polycyclic aromatic hydrocarbons in edible vegetable oil by GC-MS[J].Jiangsu Agric Sci,2014,42(11):339-341.
[13]Surma M,Sadowska-Rociek A,Cie?lik E.The application of d-SPE in the QuEChERS method for the determination of PAHs in food of animal origin with GC-MS detection[J].Eur Food Res Technol,2014,238(6):1029-1036.
[14]Madureira TV,Velhote S,Santos C,et al.A step forward using QuEChERS(quick,easy,cheap,effective,rugged,and safe)based extraction and gas chromatography-tandem mass spectrometry-levels of priority polycyclic aromatic hydrocarbons in wild and commercial mussels[J].Environ Sci Pollut R,2014,21(9):6089-6098.
[15]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-化学分册,2016,52(9):1017-1021.Lv AJ,Shi L,Cai XH,et al.QuEChERS-high performance liquid chromatography for rapid determination of 16 polycyclic aromatic hydrocarbons in rice and soil[J].Phys Chem Anal B,2016,52(9):1017-1021.
[16]Lucas LZD.PAH analysis in salmon with enhanced matrix removal-lipid[J].Food Test Agric Environ,2015.https://www.agilent.com/cs/library/applications/5991-6088EN.pdf
[17]Olsson P,Sadiktsis I,Holmb CJ,et al.Class separation of lipids and polycyclic aromatic hydrocarbons in normal phase high performance liquid chromatography-A prospect for analysis of aromatics in edible vegetable oils and biodiesel exhaust particulates[J].J Chromatogr A,2014,1360:39-46.
[18]方杰,王凯雄.气相色谱-离子阱质谱法测定海洋贝类中多残留有机氯农药、多氯联苯和多环芳烃[J].分析化学,2007,35(11):1607-1613.Fang J,Wang KX.Determination of polychlorinated pesticides,polychlorinated biphenyls and polycyclic aromatic hydrocarbons in marine shellfish by gas chromatography-ion trap mass spectrometry[J].Anal Chem,2007,35(11):1607-1613.
[19]孙红梅,朱玉梅,周军.GC/MS/MS法测定土壤中16种多环芳烃的仪器条件[J].环境与发展,2017,29(7):132-134.Sun HM,Zhu YM,Zhou J.Instrumental conditions for the determination of 16 polycyclic aromatic hydrocarbons in soil by GC/MS/MS[J].Environ Dev,2017,29(7):132-134.
[20]周华,张蕴,张喆骅,等.高分子印迹固相萃取技术结合GC/MS法测定食用油中16种多环芳烃[J].卫生研究,2016,(6):957-962.Zhou H,Zhang Y,Zhang ZH,et al.Determination of 16 polycyclic aromatic hydrocarbons in edible oil by polymer imprinted solid phase extraction and GC/MS[J].J Hyg Res,2016,(6):957-962.
[21]吴性良,朱万森,马林.分析化学原理[M].北京:化学工业出版社,2010.Wu XL,Zhu WS,Ma L.Principles of analytical chemistry[M].Beijing:Chemical Industry Press,2010.