Zhang Xiaoting, Zhang Jing, Li Wenqi, Yang Yixin, Qin Peige, Zhang Xuebin, Lu Minghua
a Institute of Environmental and Analysis Science , School of Chemistry and Chemical Engineering, Henan University , Kaifeng Henan , China.
b Key laboratory of Plant Stress Biology, State Key Laboratory of Cotton Biology , School of Life Sciences, Henan University , Kaifeng China.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018 Nov;35(11):2099-2110. doi: 10.1080/19440049.2018.1526415. Epub 2018 Oct 23.
This work presents a method of magnetic solid-phase extraction (MSPE) combined with high-performance liquid chromatography (HPLC) to analyse five synthetic azo dyes (tartrazine, amaranth, carmine, sunset yellow, allura red) in different food samples. The magnetic graphene oxide nanocomposite (GO@FeO) was prepared by a one-step solvothermal method and used as the sorbent for extraction and pre-concentration of azo dyes in food samples. The as-prepared GO@FeO nanocomposite was characterised by transmission electron microscope, Fourier transform-infrared spectroscopy, X-ray diffraction, vibrating sample magnetometer, and Brunuer-Emmett-Teller analysis. The extraction and desorption parameters were investigated, including the material amount, extraction time, pH of the solution, desorption temperature, and desorption solvents. Under the optimised conditions, the limits of detection (LODs) were 1.14-2.23, 0.36-0.77 and 0.68-1.26 ng/g for candy, jelly, and plum candy, respectively. The limits of quantification (LOQs) were 4.02-7.73, 1.21-2.50 and 2.31-4.20 ng/g for candy, jelly, and plum candy, respectively. For the analysis of spiked jelly, recoveries were between 73.2% and 107.7%, with RSDs lower than 1.34 %. The developed method was successfully applied to the analysis of real samples including jelly, candy and plum candy.
本研究提出了一种将磁性固相萃取(MSPE)与高效液相色谱(HPLC)相结合的方法,用于分析不同食品样品中的五种合成偶氮染料(柠檬黄、苋菜红、胭脂红、日落黄、诱惑红)。采用一步溶剂热法制备了磁性氧化石墨烯纳米复合材料(GO@FeO),并将其用作食品样品中偶氮染料萃取和预浓缩的吸附剂。通过透射电子显微镜、傅里叶变换红外光谱、X射线衍射、振动样品磁强计和布鲁诺尔-埃米特-泰勒分析对所制备的GO@FeO纳米复合材料进行了表征。研究了萃取和解吸参数,包括材料用量、萃取时间、溶液pH值、解吸温度和解吸溶剂。在优化条件下,糖果、果冻和酸梅糖中偶氮染料的检测限(LOD)分别为1.14 - 2.23、0.36 - 0.77和0.68 - 1.26 ng/g。糖果、果冻和酸梅糖的定量限(LOQ)分别为4.02 - 7.73、1.21 - 2.50和2.31 - 4.20 ng/g。对于加标果冻的分析,回收率在73.2%至107.7%之间,相对标准偏差低于1.34%。所建立的方法成功应用于果冻、糖果和酸梅糖等实际样品的分析。