固相萃取-高效液相色谱法测定禽类可食性组织和蛋中氨丙啉残留  

Determination of Amprolium Residues in Edible Tissues and Eggs of Poultry by Solid Phase Extraction-high Performance Liquid Chromatography

作　　者：刘畅 王蓓[3] 李康 徐坤 邱梅 程雪晴[1] 郝智慧 曲丽华[1] LIU Chang;WANG Bei;LI Kang;XU Kun;QIU Mei;CHENG Xueqing;HAO Zhihui;QU Lihua(College of Chemistry and Pharmaceutical Sciences,Qingdao Agricultural University,Qingdao 266109,China;Innovation Center for Traditional Chinese Veterinary Medicine,College of Veterinary Medicine,China Agricultural University,Beijing 100193,China;Qingdao Institute for Food Control,Qingdao 266071,China)

机构地区：[1]青岛农业大学化学与药学院,山东青岛266109 [2]中国农业大学动物医学院,中兽医药创新中心,北京100193 [3]青岛食品检验所,山东青岛266071

出　　处：《现代食品科技》2023年第6期298-305,共8页Modern Food Science and Technology

基　　金：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)。

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-6mmol/L1-庚烷磺酸钠溶液为流动相进行等度洗脱,检测波长为268nm。氨丙啉在0.1~10μg/mL呈良好的线性关系,r^(2)为0.999。该方法对鸡、鸭、鹅的肌肉中氨丙啉的检出限为150μg/kg,定量限为250μg/kg;鸡、鸭、鹅的肝脏、肾脏、脂肪、蛋中氨丙啉的检出限为250μg/kg,定量限为500μg/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。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 0.1~10μg/mL(r^(2)=0.999).The limit of detection and limit of quantification were 150μg/kg and 250μg/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 250μg/kg and 500μg/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.

关 键 词：氨丙啉 固相萃取-高效液相色谱法 残留分析 食品质量控制 

分 类 号：O657.72[理学—分析化学] TS207.3[理学—化学]