串联分子印迹固相萃取-高效液相色谱法测定食用油中苯并(a)芘
|
摘要
目的建立一种分子印迹固相萃取-高效液相色谱法测定食用油中苯并(a)芘的含量的分析方法。方法在GB 5009.27-2016《食品中苯并(a)芘的测定》试样处理方法基础上,进一步使用Welchrom~?Silica硅胶固相萃取小柱串联Welchrom~?BAP-2分子印迹固相萃取小柱对多种食用油基质进行净化。试样中目标物采用Ultimate~?XB-C_(18)(4.6 mm×250 mm, 5μm)色谱柱分离,以乙腈和水(88:12, V:V)为流动相进行等度洗脱,于激发波长370nm、发射波长425nm处进行检测。结果食用油试样经串联固相萃取小柱净化,除杂的效果好、回收率高。线性范围为1.0～100.0μg/mL,线性相关系数r在为0.9999,回收率在88.7%～101.3%之间,检出限为0.5μg/kg。结论本文建立的方法简便、灵敏度高、准确性好,适用于食品中苯并(a)芘的定性定量分析。
Objective To establish a method for determination of benzo(a)pyrene in edible oil by molecularly imprinted solid phase extraction-high performance liquid chromatography. Methods Based on the sample processing method of GB 5009.27-2016 Determination of benzo(a)pyrene in foods, Welchrom~? Silica silica solid phase extraction cartridges were connected in series with Welchrom~? BAP-2 molecularly imprinted solid phase extraction cartridges for purification several edible oil. The target in the sample was separated by a Ultimate~? XB-C_(18)(4.6 mm×250 mm, 5 μm) column. The acetonitrile and water(88:12, V:V) was used as mobile for isocratic elution,and the sample was detected at an excitation wavelength of 370 nm and an emission wavelength of 425 nm. Results The results showed that cascaded SPE column provided good impurity elimination and high recovery on cooking oil sample. The calibration curves showed a good linearity with correlation at 0.9999. The linear range for the quantification of benzo(a)pyrene were 1.0-100.0 μg/mL. The recoveries of the method were 88.7%-101.3%. The limits of detection were 0.5 μg/kg. Conclusion This method is simple, sensitive, accurate and is suitable for the quantitative analysis of the benzo(a)pyrene in edible oil samples.
Objective To establish a method for determination of benzo(a)pyrene in edible oil by molecularly imprinted solid phase extraction-high performance liquid chromatography. Methods Based on the sample processing method of GB 5009.27-2016 Determination of benzo(a)pyrene in foods, Welchrom~? Silica silica solid phase extraction cartridges were connected in series with Welchrom~? BAP-2 molecularly imprinted solid phase extraction cartridges for purification several edible oil. The target in the sample was separated by a Ultimate~? XB-C_(18)(4.6 mm×250 mm, 5 μm) column. The acetonitrile and water(88:12, V:V) was used as mobile for isocratic elution,and the sample was detected at an excitation wavelength of 370 nm and an emission wavelength of 425 nm. Results The results showed that cascaded SPE column provided good impurity elimination and high recovery on cooking oil sample. The calibration curves showed a good linearity with correlation at 0.9999. The linear range for the quantification of benzo(a)pyrene were 1.0-100.0 μg/mL. The recoveries of the method were 88.7%-101.3%. The limits of detection were 0.5 μg/kg. Conclusion This method is simple, sensitive, accurate and is suitable for the quantitative analysis of the benzo(a)pyrene in edible oil samples.
引文
[1]薛昆鹏,吴韶铭,陈宗良,等.改进固相萃取-高效液相色谱法测定食用油中苯并(a)芘[J].中国食品卫生杂志,2015,27(2):140-144.Xue KP,Wu SM,Chen ZL,et al.Detemination of benzo(a)pyrene level in cooking oil by improved solid phase extraction-high performance liquid chromatography[J].Chin J Food Hyg,2015,27(2):140-144.
[2]GB/T 5009.27-2003食品中苯并(a)芘的测定[S].GB/T 5009.27-2003 Determination of benzo(a)pyrene in foods[S].
[3]张海龙,张维,舒楠,等.高效液相色谱法定量分析菜籽油中的苯并芘[J].农产品加工,2017,440(9):26-28.Zhang HL,Zhang W,Shu N,et al.Quantitative determination of benzopyrene in rapeseed oil by high performance liquid chromatography[J].Farm Prod Proce,2017,440(9):26-28.
[4]蒋珍菊,王雁,杨巧.固相萃取-高效液相法测定芝麻油中苯并(a)芘[J].食品研究与开发,2016,37(17):111-115.Jiang ZJ,Wang Y,Yang Q.Determination of benzo(a)pyrene in sesame oil by solid-phase extraction coupled with high performance liquid chromatography[J].Food Res Dev,2016,37(17):111-115.
[5]王桂苓.高效液相色谱法测定食用植物油中苯并(a)芘的研究[J].食品安全质量检测学报,2015,6(12):5006-5010.Wang GL.Determination of benzo(a)pyrene in edible vegetable oil by high performance liquid chromatography[J].J Food Saf Qual,2015,6(12):5006-5010.
[6]吴腾,崔向云,扎木则仁,等.液相色谱法测定奶油仲苯并(a)芘的研究[J].食品安全质量检测学报,2015,6(8):3287-3291.Wu T,Cui XY,Zhamu ZR,et al.Determination of benzo(a)pyrene in cream by liquid chromatography[J].J Food Saf Qual,2015,6(8):3287-3291.
[7]王浩,杨红梅,邬雷,等.高效液相色谱-串联质谱法同时测定植物油中苯并芘与黄曲霉毒素B1,B2,G1,G2[J].分析测试学报,2014,33(8):911-916.Wang H,Yang HM,Wu L,et al.Simultaneous determination of benzo(a)pyrene and aflatoxins(B1,B2,G1,G2)in vegetable oil by high performance liquid chromatography-tandem mass spectrometry[J].JInstrum Anal,2014,33(8):911-916.
[8]张小涛,侯宏卫,陈欢,等.液相色谱串联质谱法测定卷烟主流烟气中的苯并[a]芘[J].中国烟草科学,2016,37(6):77-81.Zhang XT,Hou HW,Chen H,et al.Determination of benzo[a]pyrene in mainstream cigarette smoke by liquid chromatography tandem mass spectrometry[J].Chin Tobacco Sci,2016,37(6):77-81.
[9]刘玉兰,张小涛,赵欢欢.液相色谱-串联质谱法检测食用油脂中苯并芘[J].农业机械,2012,10(30):45-47.Liu YL,Zhang XT,Zhao HH.Determination of benzo(a)pyrene in cooking oil by liquid chromatography tandem mass spectrometry[J].Agric Mach,2012,10(30):45-47.
[10]冯寅洁,乔勇升,陈伟,等.固相萃取-超高效液相色谱荧光法检测植物油中苯并[a]芘[J].浙江大学学报(农业与生命科学版),2015,41(2):189-194.Feng YJ,Qiao YS,Chen W,et al.Determination of benzo(a)pyrene in vegetable oil by solid phase extraction-ultraperformance liquid chromatography-fluorescence detector[J].J Zhejiang Univ(Agric Life Sci),2015,41(2):189-194.
[11]程威威,汪学德,刘兵戈,等.HPLC-FLD和GC-MS测定芝麻油中苯并芘的方法比较[J].现代食品科技,2015,31(10):282-287.Chen WW,Wang XD,Liu BG,et al.Comparison of HPLC-FLD with GC-MS in estimation of benzo[a]pyrene in sesame oil[J].Mod Food Sci Technol,2015,31(10):282-287.
[12]康明芹,曹海微,田芳洁,等.凝胶色谱-超高效液相色谱测定动物油中的苯并(α)芘[J].粮食与油脂,2016,29(8):67-69.Kang MQ,Cao HW,Tian FJ,et al.Determination of benzo(a)pyrene in animal oil by gel permeation chromatography-ultra performance liquid chromatography[J].Cere Oils,2016,29(8):67-69.
[13]徐明雅,潘丹杰,金米聪.凝胶渗透色谱法测定食用植物油中苯并(a)芘[J].食品科学,2015,36(8):240-243.Xu MY,Pan DJ,Jin MC.Determination of benzo(a)pyrene in edible vegetable oils by gel permeation chromatography[J].Food Sci,2015,36(8):240-243.
[14]GB 5009.27-2016食品中苯并(a)芘的测定[S].GB 5009.27-2016 Determination of benzo(a)pyrene in foods[S].
[15]GB 2762-2017食品中污染物限量[S].GB 2762-2017 Limit of pollutants in foods[S].
[2]GB/T 5009.27-2003食品中苯并(a)芘的测定[S].GB/T 5009.27-2003 Determination of benzo(a)pyrene in foods[S].
[3]张海龙,张维,舒楠,等.高效液相色谱法定量分析菜籽油中的苯并芘[J].农产品加工,2017,440(9):26-28.Zhang HL,Zhang W,Shu N,et al.Quantitative determination of benzopyrene in rapeseed oil by high performance liquid chromatography[J].Farm Prod Proce,2017,440(9):26-28.
[4]蒋珍菊,王雁,杨巧.固相萃取-高效液相法测定芝麻油中苯并(a)芘[J].食品研究与开发,2016,37(17):111-115.Jiang ZJ,Wang Y,Yang Q.Determination of benzo(a)pyrene in sesame oil by solid-phase extraction coupled with high performance liquid chromatography[J].Food Res Dev,2016,37(17):111-115.
[5]王桂苓.高效液相色谱法测定食用植物油中苯并(a)芘的研究[J].食品安全质量检测学报,2015,6(12):5006-5010.Wang GL.Determination of benzo(a)pyrene in edible vegetable oil by high performance liquid chromatography[J].J Food Saf Qual,2015,6(12):5006-5010.
[6]吴腾,崔向云,扎木则仁,等.液相色谱法测定奶油仲苯并(a)芘的研究[J].食品安全质量检测学报,2015,6(8):3287-3291.Wu T,Cui XY,Zhamu ZR,et al.Determination of benzo(a)pyrene in cream by liquid chromatography[J].J Food Saf Qual,2015,6(8):3287-3291.
[7]王浩,杨红梅,邬雷,等.高效液相色谱-串联质谱法同时测定植物油中苯并芘与黄曲霉毒素B1,B2,G1,G2[J].分析测试学报,2014,33(8):911-916.Wang H,Yang HM,Wu L,et al.Simultaneous determination of benzo(a)pyrene and aflatoxins(B1,B2,G1,G2)in vegetable oil by high performance liquid chromatography-tandem mass spectrometry[J].JInstrum Anal,2014,33(8):911-916.
[8]张小涛,侯宏卫,陈欢,等.液相色谱串联质谱法测定卷烟主流烟气中的苯并[a]芘[J].中国烟草科学,2016,37(6):77-81.Zhang XT,Hou HW,Chen H,et al.Determination of benzo[a]pyrene in mainstream cigarette smoke by liquid chromatography tandem mass spectrometry[J].Chin Tobacco Sci,2016,37(6):77-81.
[9]刘玉兰,张小涛,赵欢欢.液相色谱-串联质谱法检测食用油脂中苯并芘[J].农业机械,2012,10(30):45-47.Liu YL,Zhang XT,Zhao HH.Determination of benzo(a)pyrene in cooking oil by liquid chromatography tandem mass spectrometry[J].Agric Mach,2012,10(30):45-47.
[10]冯寅洁,乔勇升,陈伟,等.固相萃取-超高效液相色谱荧光法检测植物油中苯并[a]芘[J].浙江大学学报(农业与生命科学版),2015,41(2):189-194.Feng YJ,Qiao YS,Chen W,et al.Determination of benzo(a)pyrene in vegetable oil by solid phase extraction-ultraperformance liquid chromatography-fluorescence detector[J].J Zhejiang Univ(Agric Life Sci),2015,41(2):189-194.
[11]程威威,汪学德,刘兵戈,等.HPLC-FLD和GC-MS测定芝麻油中苯并芘的方法比较[J].现代食品科技,2015,31(10):282-287.Chen WW,Wang XD,Liu BG,et al.Comparison of HPLC-FLD with GC-MS in estimation of benzo[a]pyrene in sesame oil[J].Mod Food Sci Technol,2015,31(10):282-287.
[12]康明芹,曹海微,田芳洁,等.凝胶色谱-超高效液相色谱测定动物油中的苯并(α)芘[J].粮食与油脂,2016,29(8):67-69.Kang MQ,Cao HW,Tian FJ,et al.Determination of benzo(a)pyrene in animal oil by gel permeation chromatography-ultra performance liquid chromatography[J].Cere Oils,2016,29(8):67-69.
[13]徐明雅,潘丹杰,金米聪.凝胶渗透色谱法测定食用植物油中苯并(a)芘[J].食品科学,2015,36(8):240-243.Xu MY,Pan DJ,Jin MC.Determination of benzo(a)pyrene in edible vegetable oils by gel permeation chromatography[J].Food Sci,2015,36(8):240-243.
[14]GB 5009.27-2016食品中苯并(a)芘的测定[S].GB 5009.27-2016 Determination of benzo(a)pyrene in foods[S].
[15]GB 2762-2017食品中污染物限量[S].GB 2762-2017 Limit of pollutants in foods[S].
© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号 地址：北京市海淀区学院路29号 邮编：100083 电话：办公室：(+86 10)66554848；文献借阅、咨询服务、科技查新：66554700 |