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    Hantzsch反应衍生-高效液相色谱法测定酒中微量甲醛

    HPLC Determination of Trace Amount of Formaldehyde in Wine Pre-derivatized by Hantzsch Reaction

    • 摘要: 提出了Hantzsch反应衍生-高效液相色谱法测定酒中的微量甲醛的方法。优化的衍生反应条件如下:① 反应体系pH为5.5;② 反应温度为50 ℃;③ 反应时间为20 min;④ 衍生剂乙酰丙酮(0.2+100)溶液用量为0.5 mL;⑤ 氯化铵溶液浓度0.5 mol·L-1。甲醛质量浓度在2~2 000 μg·L-1范围内与峰面积呈线性关系,方法的检出限(3S/N)为0.2 μg·L-1。方法用于啤酒和白酒样品的分析,加标回收率在81.2%~102%之间。

       

      Abstract: A method of HPLC for determination of trace amount of formaldehyde in wine with derivatization by Hantzsch reaction was proposed. The optimized conditions for derivatization reaction found were as follows: ① acidity of the reaction system: pH 5.5; ② temperature of reaction: 50 ℃; ③ time of reaction: 20 min; ④ amount of acetylacetone (0.2+100) solution added: 0.5 mL; ⑤ concentration of ammonium chloride solution acidity: 0.5 mol·L-1. Linear relationship between values of peak area and mass concentration of formaldehyde was kept in the range of 2-2 000 μg·L-1, with detection limit (3S/N) of 0.2 μg· L-1.The proposed method was applied to the analysis of samples of beer and white spirit, giving values of recovery by standard addition method in the range of 81.2%-102%.

       

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