柱前紫外衍生-高效液相色谱法快速测定水产品和水发食品中的甲醛  

Determination of formaldehyde in aquatic products and water-soaked foodstuffs by high performance liquid chromatography with pre-column ultraviolet derivatization

作　　者：鄢家佳 吴雨婷[1] 张静[1] 杨碧霞[1] 卜士滨 孙成均[1,2] 

机构地区：[1]四川大学华西公共卫生学院(华西第四医院),四川成都610041 [2]四川省食品安全监测与风险评估重点实验室,四川成都610041

出　　处：《现代预防医学》2014年第21期3954-3956,3998,共4页Modern Preventive Medicine

基　　金：四川大学"大学生创新创业训练计划"资助项目(20130697)

摘　　要：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 quantification of formaldehyde in foodstuffs by high performance liquid chromatography with ultraviolet derivatization. Methods After being derivatized with ethyl- acetoacetate in ammonium acetate medium （pH=6.0）, the derivatives were separated on a Cls column with methanol-water （80： 20） as mobile phase at the flow rate 1.0 ml/min and detected at 375 nm. Results The linear range was good within 0.01-10.00 μg/ml （r〉0.999）. The detection limit （S/N=3） was 0.0015 μg/ml and the quantification limit （S/N=10） was 0.005 μg/ml. The recovery of the method was 83.2%-99.6% and RSDs （n=6） was 4.55%-6.24%, respectively. And then, the method was applied to the determination of formaldehyde in aquatic products, water-soaked products, and poultry blood-derived foods. Formaldehyde was detected in 13 samples with the content of 2.99-11.4 mg/kg. Conclusion The proposed method is simple, fast, sensitive and accurate. It is applicable for the analysis of formaldehyde in foods.

关 键 词：食品 甲醛 高效液相色谱法 柱前紫外衍生 

分 类 号：R115[医药卫生—公共卫生与预防医学]