气相色谱-质谱法测定食用槟榔中多环芳烃
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摘要
建立了测定食用槟榔中15种多环芳烃(PAHs)的气相色谱-质谱(GC-MS)的方法。样品经正己烷超声萃取后,采用凝胶渗透色谱(GPC)和分散固相萃取(DSPE)进行净化,用气相色谱-质谱(GC-MS)测定。在优化条件下,采用外标法测定,被测目标在线性范围内其相关系数(r2)不低于0.996,检出限为0.2 ng/m L~1.0 ng/m L;精密度(RSD,n=7)不大于4.38%,回收率试验结果满意。该方法用于食用槟榔中多环芳烃的测定是可行的。
A gas chromatography-mass spectrometry(GC-MS)method was developed for the determination of fifteen polycyclic aromatic hydrocarbons(PAHs)in edible betelnet.The analytes were extracted ultrasonically from edible betelnet samples by hexane,and purified by gel permeation chromatography(GPC)and dispersion solid phase extraction(DSPE),then analyzed by GC-MS with external standard method.Under the optimized conditions,the correlation coefficients(r2)of PAHs in linear range were not less than 0.996,the limits of detection were 0.2 ng/m L-1.0 ng/m L and the relative standard deviations(RSD)were lower than 4.38 %.the result of recoveries were satisfied.The results showed that the method is feasible for analysis on PAHs in edible betelnet.
A gas chromatography-mass spectrometry(GC-MS)method was developed for the determination of fifteen polycyclic aromatic hydrocarbons(PAHs)in edible betelnet.The analytes were extracted ultrasonically from edible betelnet samples by hexane,and purified by gel permeation chromatography(GPC)and dispersion solid phase extraction(DSPE),then analyzed by GC-MS with external standard method.Under the optimized conditions,the correlation coefficients(r2)of PAHs in linear range were not less than 0.996,the limits of detection were 0.2 ng/m L-1.0 ng/m L and the relative standard deviations(RSD)were lower than 4.38 %.the result of recoveries were satisfied.The results showed that the method is feasible for analysis on PAHs in edible betelnet.
引文
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[2]王丽,金芬,李敏洁,等.分散固相萃取-气相色谱-串联质谱法测定蔬菜中多环芳烃及卤代多环芳烃[J].分析化学,2013,41(6):869-875
[3]A Dugay,C Herrenknecht,M Czok,et al.New procedure for selective extraction for polycyclic aromatic hydrocarbons in plants for gas chromatographic-mass spectrometric analysis[J].Journal of Chromatography A,2002,958:1-7
[4]聂静,钱岩,段小丽,等.食品中多环芳烃的健康危害及防治措施[J].环境与可持续发展,2009(4):38-41
[5]海南省质量技术监督局.DB43 132-2004.食用槟榔[S].
[6]农业部农垦局.NY/T 487-2002.槟榔干果[S].北京:中国标准出版社,2002
[7]何秀芬,罗金辉,陈歆,等.气质联用法测定干槟榔中苯并(a)芘含量[J].热带农业科学,2012,32(1):61-64
[8]中华人民共和国卫生部.GB/T 5009.27-2003.食品中苯并(a)芘的测定[S].北京:中国标准出版社,2004
[9]国家粮食局.GB/T 22509-2008.动物油脂苯并(a)芘的测定反相高效液相色谱法[S].北京:中国标准出版社,2009
[10]中华人民共和国农业部渔业局.SC/T 3042-2008.水产品中16中多环芳烃的测定气相色谱-质谱法[S].北京:中国标准出版社,2004
[11]中华人民共和国国家质量监督检验检疫局.GB/T 23213-2008.植物油中多环芳烃的测定气相色谱-质谱法[S].北京:中国标准出版社,2009
[12]国家粮食局.GB/T 24893-2010.动植物油脂多环芳烃的测定[S].北京:中国标准出版社,2010
[13]曾浩.海洋鱼组织中多环芳烃的分析方法研究[D].北京:北京化工大学,2011