[关键词]
[摘要]
该文建立了固相萃取-高效液相色谱法检测鸡、鸭、鹅的可食性组织(肌肉、肝脏、肾脏、脂肪)和蛋中氨丙啉残留的分析方法。样品中的氨丙啉经三氯乙酸-乙腈溶液提取,固相萃取柱净化。色谱柱为亲水性C18色谱柱,使用甲醇-乙腈-6 mmol/L 1-庚烷磺酸钠溶液为流动相进行等度洗脱,检测波长为268 nm。氨丙啉在0.1~10 μg/mL呈良好的线性关系,r2为0.999。该方法对鸡、鸭、鹅的肌肉中氨丙啉的检出限为150 μg/kg,定量限为250 μg/kg;鸡、鸭、鹅的肝脏、肾脏、脂肪、蛋中氨丙啉的检出限为250 μg/kg,定量限为500 μg/kg。这些空白组织中添加水平分别为定量限0.5倍、1倍、2倍最大残留限量时,各组织中氨丙啉的平均回收率在74.65%~96.24%之间,其日内和日间相对标准偏差分别小于15%。该方法准确度和精密度高,适用于禽类可食性组织和蛋中氨丙啉残留的检测,为日常工作中食品质量控制提供了一种可行的方法。
[Key word]
[Abstract]
An analytical method based on solid phase extraction-high performance liquid chromatography was established for the determination of amprolium residues in the edible tissues (muscle, liver, kidney, and fat) and eggs of chicken, ducks, and geese. First, amprolium in the sample was extracted by trichloroacetic acid-acetonitrile solution and purified by the solid-phase extraction column. A hydrophilic C18 chromatographic column was used; methanol, acetonitrile, and 6 mmol/L sodium 1-heptanesulfonate solution were used as the mobile phase for isocratic elution, with a detection wavelength of 268 nm. Amprolium exhibited an optimum linear relationship in the range of 0.1~10 μg/mL (r2=0.999). The limit of detection and limit of quantification were 150 μg/kg and 250 μg/kg, respectively, for amprolium in chicken, ducks, and geese muscle, whereas the limit of detection and limit of quantification of amprolium in the liver, kidney, fat, and eggs of chicken, ducks, and geese were 250 μg/kg and 500 μg/kg, respectively. When the addition levels in the blank tissues had a limit of quantification 0.5, 1, and 2 times the maximum residue limit, the average recoveries of amprolium ranged from 74.65%~96.24% and the intra-day and inter-day relative standard deviations were less than 15%. This method has high accuracy and precision, and is suitable for determining amprolium residues in the edible tissues and eggs of poultry, providing a feasible method for ensuring food quality control in routine applications.
[中图分类号]
[基金项目]
农业行业标准制定和修订项目(662/2319043);山东省重点研发计划项目(2019GSF107073);山东省双百计划项目(WST2017010)