【作者】 暴永康； 王丽娟； 张志强； 安东各； 涂光忠；

【Author】 Kangyong Bao;Lijuan Wang;Zhiqiang Zhang;Dongge An;Guangzhong Tu;Beijing institute of microchemistry;

【机构】 北京微量化学研究所；

【摘要】 当前社会上保健品中非法添加功能性物质引发的食品安全问题日益突出,常规检测方法不足以实现准确、及时的分析。本文采用NMR脉冲宽度定量(PULCON)技术,建立了定量检测保健品内非法添加物的方法体系。该方法通过分别测定已知浓度定量外标物和被测物的90°脉冲宽度、定量峰峰面积,得到样品中被测物的绝对含量。本实验研究对象为甲苯磺丁脲和市售保健品。以马来酸为外标物,选择合适的溶剂和定量特征峰,优化脉冲宽度、扫描间隔时间、扫描次数等实验参数。结果表明:甲苯磺丁脲的质量浓度在0.1011~4.044mg/mL内线性良好,其线性回归方程及相关系数为y=1.044x-0.003,R2=0.999;回收率为99%~102%,与NMR内标法相比,结果相近;精密度RSD均小于2%;定量限为0.1011mg/mL,检出限为0.0101mg/mL;对市售保健品检测发现,与HPLC结果接近。该方法简单、快速、可避免内标选择困难问题等,实现保健品内非法添加物的无内标、无标准品的绝对定量检测,为食品安全监控工作提供有力的技术支持。更多还原

【Abstract】 A quantitative NMR method had been established for determination of illegal functional component in dietary supplements based on PULCON principle. The optimized parameters in the PULCON method includes solvent, pulse width, the main quantitative characteristic peaks, number of scan and so on. The result indicates that the calibration curves of tolbutamide showed good linearity in the concentration range of 0.1011~4.044mg/mL. the linear regression equation and the correlation coefficients were y=1.044x-0.003,R2 = 0.999,respectively. The recoveries were 99%~102% which was in agreement with NMR quantification using internal standard. The RSD of within-day and day to day were lower than 2%. For the tolbutamide, the detection limit of the method was 0.0101mg/mL, the limit of quantitation was 0.1011mg/mL. After the analysis of sample, the RSD of the PULCON was close to the HPLC’s. The method achieved absolute determination without reference and external standard, but also provided a powerful technique for food safety detection.更多还原