以已知浓度的柠檬酸作为定量外标,琥珀酸和烟酰胺分别作为定量内标,建立了食品中水苏糖的核磁共振定量分析检测方法。该方法在0.025~6.40 g/L质量浓度范围内线性良好,相关系数R2>0.999;以柠檬酸作为外标方法加标回收率为97.91%,日内精密度与日间精密度分别为1.65%和5.27%;琥珀酸和烟酰胺作为内标方法加标回收率分别为101.39%和106.35%,日内精密度分别为1.34%和0.83%,日间精密度分别为0.65%和2.46%;对市售不同食品基质(固态、液态)中水苏糖含量进行检测,测定结果准确。与现行行业标准(QB/T 4260—2011)高效液相色谱法相比,该方法简化了样品的前处理操作,节约了时间,定量准确,对食品中水苏糖的定量检测具有更广泛的适用性。
A method to quantify stachyose in foods using nuclear magnetic resonance (NMR) was established in this study using known concentration of citric acid as an external standard, and succinic acid and nicotinamide as internal standards. For this method, a good linearity was observed in the concentration range of 0.025-6.40 g/L (R2>0.999). The recovery rate of citric acid was 97.91%, and the intra-day and inter-day precisions were 1.65% and 5.27%, respectively. The recovery rates of succinic acid and nicotinamide were 101.39% and 106.35%, respectively. Besides, the intra-day precisions for succinic acid and nicotinamide were 1.34% and 0.83%, respectively, and the inter-day precisions were 0.65% and 2.46%, respectively. The stachyose content in different solid and liquid commercial samples were tested, and the results were accurate and reliable. Compared with methods that are currently used in industries based on HPLC (QB/T 4260—2011), this method simplified sample pretreatment, saved time, quantified accurately, and had wider applicability for quantitative detection of stachyose in foods.
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