钴铁氧体磁性固相萃取结合高效液相色谱法测定果蔬汁中4种人工合成色素

doi:10.3969/j.issn.1000-1565.2019.01.008

河北大学学报(自然科学版) ›› 2019, Vol. 39 ›› Issue (1): 41-48.DOI: 10.3969/j.issn.1000-1565.2019.01.008

钴铁氧体磁性固相萃取结合高效液相色谱法测定果蔬汁中4种人工合成色素

李兴红,江静,杨莉纳,李美婷,何怡凡,张红医,石志红

收稿日期:2018-03-21 出版日期:2019-01-25 发布日期:2019-01-25
通讯作者: 石志红(1968—),女,河北保定人,河北大学教授,博士,主要从事分离科学及食品安全研究. E-mail:shizhihong@hbu.edu.cn
作者简介:李兴红(1989—),女,河北石家庄人,河北大学在读硕士研究生,主要从事色谱分析研究. E-mail:lixinghong0702@163.com
基金资助:
教育部留学回国人员科研启动基金(47批);河北大学研究生创新资助项目(hbu2018ss21);河北大学2018年实验室开放项目(sy201801);河北大学2018年校级大学生创新创业计划训练项目

Cobalt ferrite based magnetic solid phase extraction coupled with HPLC for the determination of four kinds of synthetic colourants in fruit and vegetable juices

LI Xinghong, JIANG Jing, YANG Lina, LI Meiting, HE Yifan, ZHANG Hongyi, SHI Zhihong

Key Laboratory of Analytical Science and Technology of Hebei Province, College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China

Received:2018-03-21 Online:2019-01-25 Published:2019-01-25

摘要/Abstract

摘要： 以钴铁氧体(CoFe₂O₄)作为磁性固相萃取(MSPE)的吸附剂,建立了MSPE-HPLC-UV检测果蔬汁中人工合成色素柠檬黄、胭脂红、日落黄、诱惑红的分析方法. 采用溶剂热法制备了CoFe₂O₄,通过TEM及FT-IR对其进行表征.在酸性条件下,表面呈正电性的CoFe₂O₄与含磺酸基的合成色素主要通过静电作用相互结合,从而实现目标物的萃取. 实验对材料类型和用量、溶液pH值、萃取时间等条件进行了优化. 在最佳条件下,4种色素在0.04~2.0 μg/mL内峰面积与质量浓度呈良好的线性关系,加标回收率在85.6%~106.6%之间,检出限为0.005~0.011 μg/mL. 最终将该方法用于测定果蔬汁中的合成色素,结果表明该方法快速灵敏,回收率较高,适用于实际样品中合成色素的检测.

关键词: 人工合成色素, 钴铁氧体, 磁性固相萃取, 高效液相色谱法, 果蔬汁

Abstract: A novel magnetic solid phase extraction method based on cobalt ferrite(CoFe₂O₄)as adsorbent was developed for the HPLC determination of tartrazine, sunset yellow, carmine and allure red in fruit and vegetable juice. The magnetic nanoparticles were prepared via solvothermal method and characterized by transmission electron microscope(TEM)and Fourier transform infrared spectrometer(FT-IR). The analytes were adsorbed by the magnetic microspheres due to hydrophobic and electrostatic interaction under acidic condition. Several important parameters affecting the extraction efficiency, such as the type and amount of adsorbent, pH, extraction temperature and time, type and amount of desorption solvent, - DOI:10.3969/j.issn.1000-1565.2019.01.008钴铁氧体磁性固相萃取结合高效液相色谱法测定果蔬汁中4种人工合成色素李兴红,江静,杨莉纳,李美婷,何怡凡,张红医,石志红(河北大学化学与环境科学学院,河北省分析科学技术重点实验室,河北保定 071002)摘要:以钴铁氧体(CoFe₂O₄)作为磁性固相萃取(MSPE)的吸附剂,建立了MSPE-HPLC-UV检测果蔬汁中人工合成色素柠檬黄、胭脂红、日落黄、诱惑红的分析方法. 采用溶剂热法制备了CoFe₂O₄,通过TEM及FT-IR对其进行表征.在酸性条件下,表面呈正电性的CoFe₂O₄与含磺酸基的合成色素主要通过静电作用相互结合,从而实现目标物的萃取. 实验对材料类型和用量、溶液pH值、萃取时间等条件进行了优化. 在最佳条件下,4种色素在0.04~2.0 μg/mL内峰面积与质量浓度呈良好的线性关系,加标回收率在85.6%~106.6%之间,检出限为0.005~0.011 μg/mL. 最终将该方法用于测定果蔬汁中的合成色素,结果表明该方法快速灵敏,回收率较高,适用于实际样品中合成色素的检测.关键词:人工合成色素;钴铁氧体;磁性固相萃取;高效液相色谱法;果蔬汁中图分类号:O658 文献标志码:A 文章编号:1000-1565(2019)01-0041-08Cobalt ferrite based magnetic solid phase extraction coupled with HPLC for the determination of four kinds of synthetic colourants in fruit and vegetable juicesLI Xinghong, JIANG Jing, YANG Lina, LI Meiting, HE Yifan, ZHANG Hongyi, SHI Zhihong(Key Laboratory of Analytical Science and Technology of Hebei Province, College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China)Abstract:A novel magnetic solid phase extraction method based on cobalt ferrite(CoFe₂O₄)as adsorbent was developed for the HPLC determination of tartrazine, sunset yellow, carmine and allure red in fruit and vegetable juice. The magnetic nanoparticles were prepared via solvothermal method and characterized by transmission electron microscope(TEM)and Fourier transform infrared spectrometer(FT-IR). The analytes were adsorbed by the magnetic microspheres due to hydrophobic and electrostatic interaction under acidic condition. Several important parameters affecting the extraction efficiency, such as the type and amount of adsorbent, pH, extraction temperature and time, type and amount of desorption solvent, - 收稿日期:2018-03-21 基金项目:教育部留学回国人员科研启动基金(47批);河北大学研究生创新资助项目(hbu2018ss21);河北大学2018年实验室开放项目(sy201801);河北大学2018年校级大学生创新创业计划训练项目第一作者:李兴红(1989—),女,河北石家庄人,河北大学在读硕士研究生,主要从事色谱分析研究. E-mail:lixinghong0702@163.com 通信作者:石志红(1968—),女,河北保定人,河北大学教授,博士,主要从事分离科学及食品安全研究. E-mail:shizhihong@hbu.edu.cn第1期李兴红等:钴铁氧体磁性固相萃取结合高效液相色谱法测定果蔬汁中4种人工合成色素were investigated. Under the optimized conditions, good linearity was achieved in the range from 0.04 to 2.0 μg/mL. The limits of detection for the established method were in the range of 0.005~0.011 μg/mL. The recoveries of the four synthetic colourants ranged from 85.6% to 106.6%. The established method has been proven to be successful for the determination of the four synthetic colourants in real samples.

Key words: synthetic colourant, cobalt ferrite(CoFe₂O₄), magnetic solid phase extraction(MSPE), high performance liquid chromatography(HPLC), fruit and vegetable juices

中图分类号:

O658

李兴红,江静,杨莉纳,李美婷,何怡凡,张红医,石志红. 钴铁氧体磁性固相萃取结合高效液相色谱法测定果蔬汁中4种人工合成色素[J]. 河北大学学报(自然科学版), 2019, 39(1): 41-48.

LI Xinghong, JIANG Jing, YANG Lina, LI Meiting, HE Yifan, ZHANG Hongyi, SHI Zhihong. Cobalt ferrite based magnetic solid phase extraction coupled with HPLC for the determination of four kinds of synthetic colourants in fruit and vegetable juices[J]. Journal of Hebei University (Natural Science Edition), 2019, 39(1): 41-48.

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钴铁氧体磁性固相萃取结合高效液相色谱法测定果蔬汁中4种人工合成色素

Cobalt ferrite based magnetic solid phase extraction coupled with HPLC for the determination of four kinds of synthetic colourants in fruit and vegetable juices

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