高效液相色谱法检测鮰鱼体内丁香酚的残留

Determination of eugenol residues in channel catfish by high performance liquid chromatography

中文关键词:  丁香酚  斑点叉尾鮰  高效液相色谱法  残留量

英文关键词:eugenol  Ietalurus punetaus  high performance liquid chromatography  residue

中文摘要:

      目的 建立测定斑点叉尾鮰中丁香酚残留量的高效液相色谱法, 并探究高、中、低3个不同丁香酚浓度在鱼体内的残留规律。方法 样品先经过冷冻干燥法将鱼肉冻干, 磨成粉状过筛, 称0.5 g冻干鱼粉经5 mL乙腈超声重复提取3次, 280 nm条件下, 高效液相色谱技术进样检测, 采用外标法定量。结果 丁香酚标样在0.15~20.0 mg/L浓度范围内, 线性关系良好, 线性相关系数达到0.99996。在添加浓度为0.40-3.20 mg/kg时, 加标回收率在78.67%~90.54%, 相对标准偏差为3.37%~5.54%, 方法的检出限为0.045 mg/kg。同时发现麻醉时所用的丁香酚溶液浓度越高, 丁香酚在鱼体内积累越多, 用60 mg/L丁香酚溶液麻醉过的鮰鱼, 体内丁香酚完全代谢需6~8 d, 而用40、16 mg/L丁香酚溶液麻醉过的鮰鱼, 仅需4~6 d。结论 本方法具有操作简便、快速、准确、所用试剂价格低廉的特点, 适用于斑点叉尾鮰中丁香酚残留量批量检测。

英文摘要:

      Objective To establish a method for the determination of eugenol residues in channel catfish by high performance liquid chromatography (HPLC), and investigate the residues of eugenol in fish at 3 different concentrations. Methods The flesh of fish was frozen-dried by freeze dryer, grinded into powder and sifted. The 0.5 g frozen-dried sample was extracted by 5 mL acetonitrile ultrasound for 3 times. Under 280 nm conditions, the samples were detected by high performance liquid chromatography and quantified by external standard method. Results Eugenol standard samples had a good linear relationship within the concentration range of 0.15-20.0 mg/L, and the linear correlation coefficient reached 0.99996. When the added concentration was 0.40-3.20 mg/kg, the recoveries were 78.67%-90.54%, with the relative standard deviation were 3.37%-5.54%, and the limit of detection was 0.045 mg/kg. At the same time, it was also found that the higher the concentration of eugenol solution used during anesthesia, the more eugenol accumulated in the fish. With 60 mg/L of eugenol solution anesthetizing the fish, the metabolism of eugenol totally takes 6-8 d, and with 40, 16 mg/L of eugenol solution anesthetizing the fish, only 4-6 d. Conclusion This method is simple, rapid, accurate and cheap, which is suitable for the batch detection of eugenol residues in catfish.