Yugao Guo , Xiaoxiao Niu , Boyu Li , Pei Liu , Youqing Sun , Sumin Lu
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引用次数: 0
摘要
本研究成功合成了一种聚多巴胺包覆磁铁矿/二氧化硅复合材料(Fe3O4@SiO2/PDA),并利用傅里叶变换红外光谱(FT-IR)、x射线衍射(XRD)和x射线光电子能谱(XPS)对其进行了表征。将EM-MSPE与高效液相色谱(HPLC)相结合,建立了灵敏、准确测定苏丹红I-IV染料的EM-MSPE-HPLC新方法。对吸附剂用量、pH、无机盐浓度、吸附时间、电压、洗脱液类型、洗脱液体积、脱附时间等关键实验参数进行了系统的考察和优化。在最佳条件下,该方法具有良好的线性(R²>;0.999),浓度范围为5-1000 μg L -⁻¹,检测限(lod)范围为0.11至0.17 μg L -⁻¹。苏丹红染料在实际样品中的回收率为89.1 % ~ 101.9 %,相对标准偏差(rsd)为0.3 % ~ 3.6 %。此外,Fe3O4@SiO2/PDA吸附剂在连续10次萃取循环中表现出一致的性能,且回收率没有明显下降。这些结果表明,该方法准确、可靠、可重复性好,可用于复杂饮料基质中苏丹红染料的同时测定,为食品安全应用提供了可靠的分析方法。
Magnetic solid-phase extraction of Sudan dyes from beverages-coated magnetite/silica materials
In this study, a polydopamine-coated magnetite/silica composite material (Fe3O4@SiO2/PDA) was successfully synthesized and characterized using Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). By integrating EM-MSPE with high-performance liquid chromatography (HPLC), a novel EM-MSPE-HPLC method was established for the sensitive and accurate determination of Sudan I-IV dyes. Key experimental parameters, such as adsorbent dosage, pH, inorganic salt concentration, adsorption time, voltage, eluent type, eluent volume, and desorption time, were systematically investigated and optimized. Under optimal conditions, the method demonstrated excellent linearity (R² > 0.999) within a concentration range of 5–1000 μg L⁻¹, with limits of detection (LODs) ranging from 0.11 to 0.17 μg L⁻¹. The recoveries of Sudan dyes in real samples ranged from 89.1 % to 101.9 %, with relative standard deviations (RSDs) between 0.3 % and 3.6 %. Furthermore, the Fe3O4@SiO2/PDA adsorbent exhibited consistent performance over ten consecutive extraction cycles without significant loss in recovery efficiency. These findings demonstrate that the proposed method is accurate, reliable, and reproducible for the simultaneous determination of Sudan dyes in complex beverage matrices, offering a robust analytical approach for food safety applications.