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针对奶糖及奶制品的甲醛残留问题,建立了一种灵敏、快速和有效的HPLC-UV检测乳制品中甲醛的方法。牛奶和奶粉样品中甲醛经三氯乙酸(TCA)提取,奶糖另添加乙酸锌和亚铁氰化钾进行辅助沉淀,用1mg/mL2,4-二硝基苯肼(DNPH),在60℃条件下衍生30min后,用HPLC-UV分离测定,外标法定量。该方法对3种奶制品平均加标回收率在95%以上,日内精密度和日间精密度在5%以下,甲醛含量在0.03～4.00μg/mL范围内呈良好的线性关系,检出限和定量限分别为0.03μg/mL和0.10μg/mL,对常见醛类和醇类有较好的抗干扰性。该方法具有操作简单,准确性高,稳定性好,抗干扰性强的特点,是一种测定乳制品中甲醛的有效分析技术。
Aiming at the problem of residual formaldehyde in milk sugar and dairy products, a sensitive, rapid and effective HPLC-UV method for the determination of formaldehyde in dairy products was established. Formaldehyde in milk and milk powder samples were extracted with trichloroacetic acid (TCA), toffee supplemented with zinc acetate and potassium ferrocyanide to aid in precipitation, and 1 mg / mL 2,4-dinitrophenylhydrazine (DNPH) After derivatization for 30min under conditions, it was determined by HPLC-UV separation and external standard method. The average recoveries of the three kinds of dairy products were above 95%. The intra-day precision and intra-day precision were below 5% and the formaldehyde content was within the range of 0.03-4.00 μg / mL. The detection limit And the limit of quantification were 0.03 μg / mL and 0.10 μg / mL, respectively, with good anti-interference to common aldehydes and alcohols. The method has the advantages of simple operation, high accuracy, good stability and strong anti-interference, and is an effective analytical technique for the determination of formaldehyde in dairy products.