衍生化反相高效液相色谱法检测水产品中的甲醛残留量  

Determination of Formaldehyde Residues in Aquatic Products with Derivatization Reversed-Phase High Performance Liquid Chromatography

作　　者：徐继松 翟少伟 许璐 刘宏伟 李忠琴 XU Jisong;ZHAI Shaowei;XU Lu;LIU Hongwei;LI Zhongqin(Engineering Research Center of the Modern Technology for Eel Industry,Ministry of Education,P.R.China,Xiamen 361021)

机构地区：[1]集美大学水产学院鳗鲡现代产业技术教育部工程研究中心

出　　处：《食品工业》2019年第10期299-303,共5页The Food Industry

基　　金：“十三五”厦门市海洋经济创新发展示范项目（16CZB020SF11）;现代农业产业技术体系专项资金（CARS-46）;鳗鲡现代产业技术教育部工程研究中心开放基金（RE201606）;大学生创新训练计划（201710390263）

摘　　要：建立了衍生化反相高效液相色谱法测定水产品中甲醛含量,开展水产品甲醛残留量的调查。优化样品前处理条件,经三氯乙酸结合超声的方式提取甲醛,在60℃水浴下与2,4-二硝基苯肼进行衍生化反应;通过液相色谱定量制作两条标准曲线:Y=28.387X+12.018和Y=38.8X+2.0771,线性范围分别为1~15μg/mL和0.1~1μg/mL,相关系数R分别为0.9999和0.9992;该方法的检出限为0.046 mg/kg;试样的平均回收率为101.25%(加标浓度为48.3,64.4和80.5 mg/kg)和84.57%(加标浓度为0.995,2.49和4.98 mg/kg),精密度(n=7)分别达到0.65%和0.42%,说明检测的准确性和重复性良好,能满足甲醛残留量的检测。抽检70种水产品的合格率为94.3%,与2017年国家抽验的各类水产品合格率结果接近。A derivatization reversed-phase high performance liquid chromatography(RP-HPLC)method was used to determine formaldehydein aquatic products.The pretreatment conditions of the aquatic products were optimized.The samples were extracted bytrichloroacetic acid combined with ultrasonic method.The samples were derived with 2,4-dinitrophenylhydrazine at 60℃in a water bath.Two linear standard curves were quantitatively made with this method of RP-HPLC.The equation of standard curves were Y=28.387 X+12.018 and Y=38.8 X+2.0771,respectively,and their linearity ranges were 1-15μg/mL and 0.1-1μg/mL,respectively.The correlation coefficients were 0.9999 and 0.9992,respectively.The detection limit of this method was 0.046 mg/kg.The average recoveries of standard addition were 101.25%(standard additive concentrations were 48.3,64.4 and 80.5 mg/kg)and 84.57%(standard additive concentrations were 0.995,2.49 and 4.98 mg/kg).The RSD reached 0.65%and 0.42%(n=7),respectively.It proved that the accuracy and repeatability of the method were good,and it could satisfy the determination of formaldehyde residue.70 kinds of aquatic products were randomly selected,and the qualified rate was 94.3%.The results were close to the qualified rates of the aquatic products tested by government departments in 2017.

关 键 词：水产品 甲醛 高效液相色谱法 

分 类 号：TS2[轻工技术与工程—食品科学与工程]