牛组织中氨丙啉残留的HPLC检测方法研究

Determination of Amprolium Residues in Bovine Tissues by HPLC

关键词:  氨丙啉  残留  高效液相色谱

Key words:  amprolium, residues, HPLC

摘要:

建立了牛组织中氨丙啉残留检测的高效液相色谱法。试样中的氨丙啉经乙腈提取后旋转蒸干，用磷酸盐缓冲液溶解，过HLB固相萃取小柱净化，高效液相色谱法进行测定。结果表明，在0.20~20.0 μg/mL范围内，氨丙啉浓度与峰面积呈良好线性关系（r²=0.9999）；在牛的肌肉、肝脏、肾脏和脂肪中，氨丙啉的检测限为100 μg/kg，在牛的肌肉、肝脏、肾脏中定量限为250 μg/kg，在牛的脂肪中定量限为200 μg/kg。在不同添加浓度下测定，氨丙啉的平均回收率为60%~110%，批内和批间变异系数均在15%以内。本方法可快速测定牛组织中氨丙啉残留量，且操作简单、灵敏度高、结果准确性高，能满足日常检测需要。

Abstract:

A high-performance liquid chromatography (HPLC) method for the determination of amprolium in bovine tissues was optimized and validated. The tissues were homogenized and extracted by acetonitrile, after rotary evaporation, the residue was dissolved by phosphate buffer, and then, solid-phase extraction (HLB) was followed. Finally, the eluate was assayed by HPLC, coplued with C18 column, and detection wavelength of 267 nm. As the results showed, the calibration graphs were linear (r²=0.9999) between 0.20 μg/mL and 20.0 μg/mL for amprolium; the limit of detection (LOD) was 100 μg/kg, and the limit of quantitation (LOQ) was 250 μg/kg, except for the fat tissues, in which the LOQ was 200 μg/kg. Recoveries of amprolium in different bovine tissues and different levels were between 60% to 110％, the coefficient of variation for within-run assays and for between-run assays were both less than 15%. It was concluded that this method was simple, sensitive and reliable for food safety.