亲水作用色谱柱-高效液相色谱法测定鸡蛋中氨丙啉的残留量
目的 建立亲水作用色谱柱-高效液相色谱法检测鸡蛋中氨丙啉残留的分析方法。方法 样品加入10 mL 5%三氯乙酸水溶液进行提取, 离心后取一半上清液过HLB柱净化。色谱柱为Poroshell 120 HILIC-Z (100 mm ×3.0 mm, 2.7 μm), 流动相为5 mmol/L乙酸铵-0.1%甲酸水溶液和乙腈, 等度洗脱, 5 mmol/L乙酸铵-0.1%甲酸水溶液:乙腈=20:80(V:V), 流速为0.4 mL/min, 进样量为20 μL, 检测波长267 nm。 结果 氨丙啉在0.35~10.0 μg/mL呈良好的线性关系, r大于0.999。方法的最低定量限为250 μg/kg。氨丙啉在250~2000 μg/kg的浓度添加水平上, 其回收率在85.0%~96.7%, 批内、批间的相对标准偏差小于6%。结论 该方法具有简便快捷、灵敏度高等特点, 适用于鸡蛋中氨丙啉的残留检测。
Objective To establish a method for determination of amprolium in egg by hydrop interaction liquid chromatography column- high performance liquid chromatography (HILIC-HPLC). Methods Amprolium was extracted with 10 mL 5% trichloroacetic acid, and the half of supernatant was purified with HLB column. The chromatography column was poroshell 120 HILIC-Z (100 mm×3.0 mm, 2.7 μm). The mobile phase was acetonitrile and 5 mmol/L ammonium acetate -0.1% formic acid water with equivalent elution, the flow rate was 0.4 mL/min, injection volume was 20 μL and detection wavelengths was 267 nm. Results Amprolium had good linear relationships in the range of 0.35?10.0 μg/mL (r2>0.999), and the limit of quantification of amprolium was 250 μg/kg. The average recoveries at 250?2000 μg/kg were 85.0%?96.7%. In day-between days batch variation coefficients were both less than 6%. Conclusion This method is simple, rapid, sensitive and accurate, which can be applied for the determination of amprolium in egg.
标题：亲水作用色谱柱-高效液相色谱法测定鸡蛋中氨丙啉的残留量
英文标题：Determination of amprolium residues in egg by hydrop interaction liquid chromatography column-high performance liquid chromatography
作者：
李丹 中国兽医药品监察所,国家兽药残留基准实验室
吴翠玲 安捷伦科技(中国)有限公司
张聪聪 安捷伦科技(中国)有限公司
张玉洁 中国兽医药品监察所,国家兽药残留基准实验室
沈昕 中国兽医药品监察所,国家兽药残留基准实验室
朱馨乐 中国兽医药品监察所,国家兽药残留基准实验室
李倩 中国兽医药品监察所,国家兽药残留基准实验室
王鹤佳 中国兽医药品监察所,国家兽药残留基准实验室
中文关键词:亲水作用色谱柱-高效液相色谱法,氨丙啉,残留,鸡蛋,
英文关键词:hydrop interaction liquid chromatography column-high performance liquid chromatography,amprolium,residues,egg,
发表日期：2019-06-12
- 文件大小:
- 4.06 MB
- 下载次数:
- 60
-
高速下载
|
|
