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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 establish a method for the determination of melamine in eel by high performance liquid chromatography. Methods The samples of eel were extracted with 1% trichloroacetic acid by ultrasonic and the lipid was diluted with 1% trichloroacetic acid in dichloromethane. The mixture was concentrated and cleaned up with a mixed cation exchange solid phase extraction cartridge. The samples were eluted with SHISEIDO CAPCELL PAK CR (1: 4) mixed liquid chromatography column, DAD detector detection. Results The linear correlation coefficient of melamine in the concentration range of 0 ~ 25μg / mL was 0.9999. The average recoveries of melamine at 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%, respectively. The detection limit (S / N = 10) was 1.55 mg / kg. Conclusion All the indexes are in line with GB / T 27404-2008 “laboratory quality control food physical and chemical testing” to confirm the technical requirements of detection methods.