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水产饲料中三聚氰胺检测方法的优化
引用本文:黄和,黄春丽,陈荷英,高平,罗林,陈宏.水产饲料中三聚氰胺检测方法的优化[J].广东海洋大学学报,2011(4):62-68.
作者姓名:黄和  黄春丽  陈荷英  高平  罗林  陈宏
作者单位:广东海洋大学食品科技学院;广东省高等学校水产品深加工重点实验室;广东省湛江市质量计量监督检测所;
基金项目:广东省科技计划项目(2009B020316002)
摘    要:通过对高效液相色谱法(HPLC)测定水产饲料中三聚氰胺含量的方法进行优化,得到最佳色谱条件和前处理方法,建立了水产饲料中三聚氰胺的检测方法。结果表明:以体积比8∶92的乙腈、庚烷磺酸钠离子对试剂为流动相,柱温40℃,流速1.2 mL/min,以波长236 nm检测;以提取液为18 mL50%(φ)乙腈水+1 mL乙酸锌+1 mL1mol/L盐酸,淋洗液3 mL水和3 mL甲醇,洗脱体积6 mL作样品前处理。三聚氰胺加标回收率为85%~100%,相对标准偏差(RSD)小于5%,线性范围为0.2 mg/L~5.0mg/L,相关系数0.999 8,方法检出限为0.2 mg/kg。

关 键 词:水产饲料  三聚氰胺  高效液相色谱法

Optimization of Testing Methods of Melamine Residues in Aquatic Feed
HUANG He,HUANG Chun-li,CHEN He-ying,GAO Ping,LUO Lin,CHEN Hong.Optimization of Testing Methods of Melamine Residues in Aquatic Feed[J].Journal of Zhanjiang Ocean University,2011(4):62-68.
Authors:HUANG He    HUANG Chun-li  CHEN He-ying  GAO Ping  LUO Lin  CHEN Hong
Institution:HUANG He1,2,HUANG Chun-li1,CHEN He-ying1,GAO Ping3,LUO Lin3,CHEN Hong3(1.Institute of Food Science and Technology of Guangdong Ocean University,Zhanjiang 524088,China,2.Key Laboratory of Aquatic Products Advanced Processing of Guangdong Higher Education Institution,3.Zhanjiang Institute of Supervision & Test on Quality & Measure,Zhanjiang 524043,China)
Abstract:Using aquatic feed as subjects,the best testing method of melamine residues were set up according to the optimal chromatographic and pre-treatment conditions by HPLC.The results showed that the optimum detecting condition was that the mobile phase was composed of 92% sodium heptanesulfonate and 8% acetonitrile,temperature was 40℃,flow rate 1.2mL/min and wavelength 236nm.The optimum extraction conditions was that extract solution included 18mL 50% acetonitrile,1mL zinc acetate and 1mL 1mol/L HCl,leacheate was 3mL water and 3mL methyl alcohol,elution volume 6mL.The coefficient of recovery of the method reached 85% ~ 100%,RSD was less than 5%,standard working line linear ranged from 0.2 mg/L to 5.0 mg/L,correlation coefficient was 0.9998,the detection limit of melamine 0.2 mg/kg.
Keywords:aquatic feed  melamine  High performance liquid chromatographic  
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