高效液相色谱法-差异加标法同时快速测定饮料中的苯甲酸、山梨酸

Simultaneous and rapid determination of benzoic acid and sorbic acid in beverages by high performance liquid chromatography-differential standard addition method

目的建立高效液相色谱法-差异加标法同时快速测定饮料中苯甲酸、山梨酸的分析方法。方法以复合蛋白饮料、果蔬饮料为样品,通过亚铁氰化钾溶液和乙酸锌溶液提取后,色谱柱为AccucoreC18柱(2.1 mm×150 mm),以甲醇-0.02 mol/L乙酸铵(5:95, V:V)为流动相梯度洗脱,采用高效液相色谱法-差异加标法测定。结果该法最佳差异加标量为10μg/g和15μg/g,在此条件下测得饮料中苯甲酸、山梨酸的质量分数分别为11.8~27.6μg/g和18.1~19.4μg/g;其回收率分别为98%~111%和94%~113%;检出限分别为1.10μg/m L、1.72μg/m L;定量限分别为3.68μg/m L、5.73μg/m L。结论该方法简便、快捷,不需绘制标准工作曲线与过柱去杂质,简化了步骤、提升了检测效率与准确性,同时也扣除了背景干扰,准确、实用,是一种新型的分析检测技术。

Objective To establish a method for the simultaneous determination of benzoic acid and sorbic acid in beverage by high performance liquid chromatography-differential standard addition method. Methods The compound protein beverage and fruit and vegetable beverage were extracted by potassium ferrocyanide solution and zinc acetate solution. The chromatographic column was Accucore C18 column(2.1 mm×150 mm). Methanol-0.02 mol/L ammonium acetate(5:95, V:V) was used as mobile phase for gradient elution. The determination was performed by high performance liquid chromatography with differential standard addition method. Results The optimal differential addition values were 10 μg/g and 15 μg/g respectively. Under this condition, the mass fractions of benzoic acid and sorbic acid in the beverage were 11.8-27.6 μg/g and 18.1-19.4 μg/g respectively. The recovery rates were 98%-111% and 94%-113% respectively. The limits of detection were 1.10 μg/mL and 1.72 μg/mL, and the limits of quantitation were 3.68 μg/mL and 5.73 μg/mL, respectively. Conclusion This method is simple and fast, and does not need to draw the standard working curve and remove impurities through the column, which simplifies the steps, improves the detection efficiency and accuracy, and also eliminates the background interference.It is accurate and practical, and is a new analysis and detection technology.