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目的建立水产品和水发食品中甲醛的乙酰乙酸乙酯柱前紫外衍生-高效液相色谱快速测定方法。方法样品经研磨匀浆后,用水浸泡提取。离心后,取上清液与乙酰乙酸乙酯在乙酸铵介质(pH=6.0)中快速反应生成具有紫外吸收的衍生物,以C18柱为分离柱,甲醇-水为流动相,以紫外检测器在375 nm波长处检测,标准曲线法定量。结果在0.01~10.00μg/ml范围内线性关系良好,相关系数为0.9994,检出限和定量限分别为0.0015μg/ml(S/N=3)和0.005μg/ml(S/N=10),方法加标回收率范围为83.2%~99.6%,相对标准偏差范围为4.55%~6.24%。用本法对水发食品、水产品和血旺等样品中的甲醛进行了测定,其中13个样品检出甲醛,含量范围为2.99~11.40 mg/kg。结论该方法操作简单、快速、灵敏、准确,可用于水产品和水发食品中甲醛的快速测定。
OBJECTIVE To establish a method for the rapid determination of formaldehyde in ethyl acetate by pre-column UV-A HPLC with high performance liquid chromatography (HPLC). Methods Samples were homogenized after grinding, soaked in water extraction. After centrifugation, the supernatant and ethyl acetoacetate were reacted rapidly in ammonium acetate medium (pH = 6.0) to generate the derivative with UV absorption. The separation was performed on a C18 column with methanol-water as the mobile phase. The UV detector At 375 nm wavelength detection, standard curve method. The results showed good linearity in the range of 0.01-10.00 μg / ml with a correlation coefficient of 0.9994. The limits of detection and quantification were 0.0015 μg / ml (S / N = 3) and 0.005 μg / ml (S / N = 10) The recoveries ranged from 83.2% to 99.6%. The relative standard deviations ranged from 4.55% to 6.24%. Formaldehyde in water-based foods, aquatic products and blood-wang samples was determined by this method. Of the 13 samples, formaldehyde was detected in the range of 2.99-11.40 mg / kg. Conclusion The method is simple, rapid, sensitive and accurate and can be used for the rapid determination of formaldehyde in aquatic products and water-based foods.