Qi Feifei, Jian Ningge, Qian Liangliang, Cao Weixin, Xu Qian, Li Jian
Key Laboratory of Environmental Medicine Engineering, Ministry of Education, School of Public Health, Southeast University, Nanjing, Jiangsu, 210009, China.
Suzhou Municipal Center for Disease Prevention and Control, Suzhou, Jiangsu, 215004, China.
Anal Bioanal Chem. 2017 Sep;409(24):5697-5709. doi: 10.1007/s00216-017-0510-8. Epub 2017 Jul 24.
A simple and efficient three-step sample preparation method was developed and optimized for the simultaneous analysis of illegal anionic and cationic dyes (acid orange 7, metanil yellow, auramine-O, and chrysoidine) in food samples. A novel solid-phase extraction (SPE) procedure based on nanofibers mat (NFsM) was proposed after solvent extraction and freeze-salting out purification. The preferred SPE sorbent was selected from five functionalized NFsMs by orthogonal experimental design, and the optimization of SPE parameters was achieved through response surface methodology (RSM) based on the Box-Behnken design (BBD). Under the optimal conditions, the target analytes could be completely adsorbed by polypyrrole-functionalized polyacrylonitrile NFsM (PPy/PAN NFsM), and the eluent was directly analyzed by high-performance liquid chromatography-diode array detection (HPLC-DAD). The limits of detection (LODs) were between 0.002 and 0.01 mg kg, and satisfactory linearity with correlation coefficients (R > 0.99) for each dye in all samples was achieved. Compared with the Chinese standard method and the published methods, the proposed method was simplified greatly with much lower requirement of sorbent (5.0 mg) and organic solvent (2.8 mL) and higher sample preparation speed (10 min/sample), while higher recovery (83.6-116.5%) and precision (RSDs < 7.1%) were obtained. With this developed method, we have successfully detected illegal ionic dyes in three common representative foods: yellow croaker, soybean products, and chili seasonings. Graphical abstract Schematic representation of the process of the three-step sample preparation.
开发并优化了一种简单高效的三步样品制备方法,用于同时分析食品样品中的非法阴离子和阳离子染料(酸性橙7、间胺黄、金胺 - O和碱性菊橙)。在溶剂萃取和冷冻盐析纯化后,提出了一种基于纳米纤维垫(NFsM)的新型固相萃取(SPE)程序。通过正交实验设计从五种功能化的NFsM中选择了优选的SPE吸附剂,并基于Box - Behnken设计(BBD)通过响应面法(RSM)实现了SPE参数的优化。在最佳条件下,目标分析物可被聚吡咯功能化聚丙烯腈NFsM(PPy/PAN NFsM)完全吸附,洗脱液直接通过高效液相色谱 - 二极管阵列检测(HPLC - DAD)进行分析。检测限(LOD)在0.002至0.01 mg/kg之间,所有样品中每种染料均具有令人满意的线性关系,相关系数(R > 0.99)。与中国标准方法和已发表的方法相比,所提出的方法大大简化,对吸附剂(5.0 mg)和有机溶剂(2.8 mL)的要求更低且样品制备速度更高(10分钟/样品),同时获得了更高的回收率(83.6 - 116.5%)和精密度(RSDs < 7.1%)。使用这种开发的方法,我们成功检测了三种常见代表性食品中的非法离子染料:黄鱼、豆制品和辣椒调味料。图形摘要三步样品制备过程的示意图