【摘要】 建立检测牛肉、牛奶中氮氨菲啶残留量的高效液相色谱法。用乙腈-甲醇(含0.125 mol/L甲酸铵)溶液(体积比50∶50)提取试样中的氮氨菲啶。提取物经40℃下蒸干、甲醇溶解和正己烷除脂后,采用ODS-3 C18色谱柱,以甲醇-0.1%(体积分数)甲酸水为流动相,梯度洗脱程序分离药物与样品基质,在380 nm的紫外检测波长下进行高效液相色谱检测。试验结果表明,氮氨菲啶在0.005~1.000μg/mL质量浓度范围内呈良好的线性关系(r>0.99)。对空白牛肉、牛奶进行20~500μg/kg的药物添加回收试验,平均回收率范围为80.3%~93.0%,日内变异系数为2.8%~5.3%,日间变异系数为4.0%~8.1%。牛肉和牛奶中氮氨菲啶的检测限分别为8和6μg/kg;定量限分别为25和20μg/kg。该方法快速、准确、灵敏,适用于牛肉、牛奶中氮氨菲啶的残留检测。更多还原

【Abstract】 A high-performance liquid chromatography(HPLC) method was developed for determination of isometamidium residue in beef and milk.Isometamidium was extracted with acetonitrile-methanol(containing 0.125 mol/L ammonium formate)(50∶50) from sample.The extracts were evaporated to dryness at 40 ℃,dissolved in methanol and then rinsed with N-hexane.Separation was performed on an ODS-3 C18 column with a gradient mobile phase of methanol and 0.1% formic acid-water,and the determination was performed with UV detection at 380 nm.The calibration curve was linearity at a range of 0.005~1.000 μg/mL for the isometamidium(r>0.99).The recoveries ranged from 80.3% to 93.0% in beef and milk at a fortified concentration of 20-500 μg/kg.The inter-day and intra-day coefficients of variation were ranged from 2.8% to 5.3% and 4.0% to 8.1%,respectively.The limit of detections(LOD) of isometamidium in beef and milk were 8 and 6 μg/kg,respectively,while the limit of quantitations(LOQ) of isometamidium in beef and milk were 25 and 20 μg/kg,respectively.It was a rapid,specific,and sensitive method for determinating isometamidium residue in beef and milk.更多还原