离子液体基磁性固相萃取-高效液相色谱法测定饮料中的合成色素

    Determination of synthetic pigments in beverages by ionic liquid based magnetic solid phase extraction-high performance liquid chromatography

    • 摘要: 国家对合成色素使用量有严格限量标准,有效萃取和测定食品中合成色素对保障食品安全有重要意义。采用红外光谱、透射电镜和振动样品磁强计等对合成的聚合离子液体修饰的磁性纳米材料的结构、形貌和磁性进行了表征,将此磁性纳米材料作为磁性固相萃取(magnetic solid-phase extraction, MSPE)吸附剂,研究了其对4种合成色素(柠檬黄、日落黄、诱惑红和亮蓝)的萃取性能,结合MSPE与高效液相色谱技术,对影响萃取效率的吸附剂用量、吸附时间、解吸时间和盐的含量等参数进行了优化。研究结果表明:根据吸附剂对典型阴/阳离子型染料的吸附结果,推断4种合成色素的有效萃取归因于吸附剂与分析物之间存在的强静电引力以及π-π和疏水作用等多重作用;在吸附剂用量为10 mg、吸附时间为20 min、解吸剂为1 mL乙腈/盐酸(体积比9∶1)和解吸时间为10 s的优化萃取条件下,4种色素具有良好的线性(决定系数为0.992 2~0.997 5),检出限(S/N=3)和定量限(S/N=10)分别为1~3 μg/L和2.5~10 μg/L;该方法能成功用于碳酸饮料健力宝和菠萝啤中合成色素的测定,3个质量浓度下(日落黄、诱惑红和亮蓝均为25、100、250 μg/L,柠檬黄为50、200、500 μg/ L)的加标回收率为71.4%~113.0%,相对标准偏差小于10.9%(n=3)。本研究为食品中合成色素的分析提供了一种很有前景的样品前处理方法。

       

      Abstract: The strict limit standards for synthetic pigments maximum usage were set in our country. To ensure food safety, effective extraction and determination of synthetic pigments in food are necessary. In this study, a poly(ionic liquid)-modified magnetic nanoparticles was synthesized and served as an adsorbent of magnetic solid-phase extraction (MSPE). The structure, morphology, and magnetic property of the adsorbent were characterized by Fourier transform infrared spectroscopy, transmission electron microscopy and vibrating sample magnetometer. The extraction performance of the adsorbent was studied for four synthetic pigments including tartrazine, sunset yellow, temptation red, and brilliant blue. According to the adsorption efficiency of typical anionic and cationic dye, the effective extraction of the adsorbent for four synthetic pigments was attributed to the strong electrostatic attraction as well as the π-π and hydrophobic interactions between the adsorbent and the analytes. The main parameters influencing the extraction efficiency, such as adsorbent amount, adsorption and desorption time, and salt addition, were optimized. Under the optimized extraction conditions, the performance and applicability of the proposed method were investigated by combining with MSPE and high-performance liquid chromatography. The four synthetic pigments had a satisfactory linearity with correlation coefficients ranged from 0.992 2 to 0.997 5. The limits of detection (S/N=3) and limits of quantitation (S/N=10) were 1-3 μg/L and 2.5-10 μg/L, respectively. The method could be successfully used for the determination of synthetic pigments in two beverages (Jianlibao and Boluopi). The relative recoveries at three different spiked levels (25, 100, and 250 μg/L for sunset yellow, temptation red and brilliant blue, 50, 200, and 500 μg/L for tartrazine) ranged from 71.4% to 113.0%, and the relative standard deviations were less than 10.9% (n=3). This work provides a promising sample preparation technique for the analysis of synthetic pigments in food.

       

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