高效液相色谱法测定鳗鱼中三聚氰胺残留量

Determination of melamine residues in eel by high performance liquid chromatography

目的建立高效液相色谱法检测鳗鱼中三聚氰胺残留量的方法。方法鳗鱼试样用1%三氯乙酸超声提取,以1%三氯乙酸饱和的二氯甲烷液液分配除脂,用混合型阳离子交换固相萃取小柱富集和净化,用SHISEIDO CAPCELL PAK CR(1:4)混合液相色谱柱分离,DAD检测器检测。结果三聚氰胺在0~25μg/m L浓度范围的线性相关系数为0.9999,加标水平在2.0、4.0、10.0 mg/kg的平均回收率分别为94.0%、95.3%、99.5%,相对标准偏差RSD(n=6)分别为2.73%、3.71%、5.79%,该方法检出限(S/N=10)为1.55 mg/kg。结论各项指标均符合GB/T 27404-2008《实验室质量控制规范食品理化检测》中检测方法确认的技术要求。

Objective To develop a method for the detection of melamine residues in eel by high performance liquid chromatography.MethodsThe sample was extracted with 1% trichloroacetic acid by ultrasonic extraction, degreased through liquid-liquid distribution with methylene chloride saturated by 1% trichloroacetic acid, enriched and purified by mixed cation exchange column. SHISEIDO CAPCELL PAK CR (1:4) mixed liquid chromatographic column was used for separation, and DAD detector was used for determination.Results The correlation coefficient in the range of 0~25μg/mL was 0.9999. The recoveries of three different concentration (2.0, 4.0, and 10.0 mg/kg) were 94.0%, 95.3%, and 99.5%, respectively. The relative standard deviations (RSD,n=6) were 2.73%, 3.71% and 5.79%. The limit of detection was 1.55 mg/kg. ConclusionAll the parameters conform to technical specificationsof GB/T 27404-2008 “Criterion on quality control of laboratories-chemical testing of food”.