[关键词]
[摘要]
为检测鲜活水产品在运输过程中,丁香酚类麻醉剂的代谢残留情况,本研究建立了同时检测斑点叉尾鮰鱼肌肉组织中6种丁香酚类化合物的高效液相色谱法。取冻干鱼肉肌肉组织用15 mL甲醇与乙腈体积比为2:1的混合溶液超声提取,100 mg疏水气相纳米二氧化硅净化,过滤处理后。流动相体积比为58%甲醇和42%的0.1%乙酸水溶液,流速为0.8 mL/min,柱温箱为35 ℃,紫外检测波长为272 nm,进样量为10 μL,外标法定量。6种丁香酚类化合物在0.02~100.0 μg/mL线性关系良好,R2均大于0.999,在三个不同水平的添加浓度下,日内平均回收率在50.52%~97.98%之间,相对标准偏差在1.25%~14.56%,方法的稳定性和重复性良好。方法的检出限在0.026~0.121 mg/kg,该检出限低于日本所规定的丁香酚残留限量标准,可以用于批量鱼样中多种丁香酚类化合物的检测。
[Key word]
[Abstract]
In order to detect the metabolic residues of eugenol anesthetics during the transportation of fresh aquatic products, a high performance liquid chromatography (HPLC) method for the simultaneous determination of six eugenol compounds in the muscle tissue of catfish (Ietalurus punetaus) was developed. The freeze-dried fish muscle tissue was ultrasonically extracted with a mixture of 15 mL methanol and acetonitrile (V/V, 2:1), purified by 100 mg of hydrophobic gas phase nano-silica, and filtered. The mobile phase was a mixture of methanol and 0.1% acetic acid solution (V/V, 58:42) with a flow rate of 0.8 mL/min and ultraviolet detection wavelength at 272 nm, the column temperature was 35 ℃, the injection volume was 10 μL, and the external standard method was developed. The linear relationship of six eugenol compounds was good in the range of 0.02~100.0 ug/mL with a linear regression coefficient more than 0.999. The average intra-recovery was between 50.52% and 97.98% and the relative standard deviation was between 1.25 and 14.56% at three different addition levels. The stability and repeatability of the method were good. The detection limit of the method is 0.026~0.121 mg/kg, which is lower than the residue limit standard of eugenol in Japan. It can be used for the detection of various eugenol compounds in fish samples in batches.
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[基金项目]
现代农业产业技术体系专项资金资助(CARS-46);湖北省科技特派员项目;湖北省农业科技创新中心项目(2019-620-000-001-036)