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
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摘要
以钴铁氧体(CoFe_2O_4)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CoFe_2O_4,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CoFe_2O_4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0.04～2.0μg/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0.005～0.011μg/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.
A novel magnetic solid phase extraction method based on cobalt ferrite(CoFe_2 O_4)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,were investigated.Under the optimized conditions,good linearity was achieved in the range from 0.04 to2.0μg/mL.The limits of detection for the established method were in the range of 0.005～0.011μg/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.
A novel magnetic solid phase extraction method based on cobalt ferrite(CoFe_2 O_4)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,were investigated.Under the optimized conditions,good linearity was achieved in the range from 0.04 to2.0μg/mL.The limits of detection for the established method were in the range of 0.005～0.011μg/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.
引文
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[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 CoFe2O4submicron 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 25synthetic 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.