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.
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
.
DOI: 10.3969/j.issn.1000-1565.2019.01.008
[1] FENG J, CERNIGLIA C E, CHEN H. Toxicological significance of azo dye metabolism by human intestinal microbiota[J]. Frontiers in Bioscience(Elite edition), 2012, 4: 568-586.
[2] 赵飞,高广慧,那海秋,等. 固相萃取-高效液相色谱-可变波长检测法同时测定调味品中甜味剂和人工合成色素[J]. 色谱, 2013, 31(5): 490-493. DOI:10.3724/SP.J.1123.2012.12012.
[3] MASONE D, CHANFORAN C. Study on the interaction of artificial and natural food colorants with human serum albumin: A computational point of view [J]. Computational Biology and Chemistry, 2015, 56: 152-158. DOI:10.1016/j.compbiolchem.2015.04.006.
[4] AXON A, MAY F E B, GAUGHAN L E, et al. Tartrazine and sunset yellow are xenoestrogens in a new screening assay to identify modulators of human oestrogen receptor transcriptional activity [J]. Toxicology, 2012, 298(1-3): 40-51. DOI:10.1016/j.tox.2012.04.014.
[5] GB2760-2014, 食品安全国家标准食品添加剂使用标准[S].
[6] DORRAJI P S, JALALI F. Electrochemical fabrication of a novel ZnO/cysteic acid nanocomposite modified electrode and its application to simultaneous determination of sunset yellow and tartrazine [J]. Food Chemistry, 2017, 227: 73-77. DOI:10.1016/j.foodchem.2017.01.071.
[7] SIERRA-ROSALES P, TOLEDO-NEIRA C, SQUELLA J A. Electrochemical determination of food colorants in soft drinks using MWCNT-modified GCEs[J]. Sensors and Actuators B: Chemical, 2017, 240: 1257-1264. DOI:10.1016/j.snb.2016.08.135.
[8] BENTO W A S, LIMA B P, PAIM A P S. Simultaneous determination of synthetic colorants in yogurt by HPLC [J]. Food Chemistry, 2015, 183: 154-160. DOI: 10.1016/j.foodchem.2015.03.050.
[9] HEIDARIZADI E, TABARAKI R. Simultaneous spectrophotometric determination of synthetic dyes in food samples after cloud point extraction using multiple response optimizations [J]. Talanta, 2016, 148: 237-246. DOI: 10.1016/j.talanta.2015.10.075.
[10] S 'AFARIKOVA M, S 'AFARIK I. Magnetic solid-phase extraction [J]. Journal of Magnetism and Magnetic Materials, 1999, 194(1-3): 108-112. DOI: 10.1016/S0304-8853(98)00566-6.
[11] HERRERO-LATORRE C, BARCIELA-GARCIA J, GARCIA-MARTIN S, et al. Magnetic solid-phase extraction using carbon nanotubes as sorbents: a review[J]. Analytica Chimica Acta, 2015, 892: 10-26. DOI:10.1016/j.aca.2015.07.046.
[12] ZHOU L, FU Q, ZHOU D, et al. Solvothermal synthesis of CoFe2O4 submicron compact spheres and tunable coercivity induced via low-temperature thermal treatment[J]. Journal of Magnetism and Magnetic Materials, 2015, 392: 22-26. DOI:10.1016/j.jmmm.2015.04.114
[13] DONG N, HE F, XIN J, et al. Preparation of CoFe2O4 magnetic fiber nanomaterial via a template-assisted solvothermal method[J]. Materials Letters, 2015, 141: 238-241. DOI:10.1016/j.matlet.2014.11.054.
[14] LI H, SUN N, ZHANG J, et al. Development of a matrix solid phase dispersion-high performance liquid chromatography-tandem mass spectrometric method for multiresidue analysis of 25 synthetic colorants in meat products[J]. Analytical Methods, 2014, 6(2): 537-547. DOI:10.1039/C3AY41664J.
[15] LIU F J, LIU C T, LI W, et al. Dispersive solid-phase microextraction and capillary electrophoresis separation of food colorants in beverages using diamino moiety functionalized silica nanoparticles as both extractant and pseudostationary phase[J]. Talanta, 2015, 132: 366-372. DOI:10.1016/j.talanta.2014.09.014.
[16] MA M, LUO X, CHEN B, et al. Simultaneous determination of water-soluble and fat-soluble synthetic colorants in foodstuff by high-performance liquid chromatography-diode array detection-electrospray mass spectrometry[J]. Journal of Chromatography A, 2006, 1103(1): 170-176. DOI: 10.1016/j.chroma.2005.11.061.
[17] UNSAL Y E, SOYLAK M, TUZEN M. Column solid-phase extraction of sunset yellow and spectrophotometric determination of its use in powdered beverage and confectionery products[J]. International Journal of Food Science & Technology, 2012, 47(6): 1253-1258. DOI:10.1111/j.1365-2621.2012.02966.x.
