液相色谱-串联质谱法测定大菱鲆鱼粉中呋喃唑酮代谢物残留

Determination of furazolidone metabolite residue in the turbot fish meal by liquid chromatography-tandem mass spectrometry

中文关键词:  呋喃唑酮  液相色谱-串联质谱法  定值  鱼粉

英文关键词:furazolidone  liquid chromatography-tandem mass spectrometry  definite value  fish meal

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)检测大菱鲆鱼粉中呋喃唑酮代谢物3-氨基-2-噁唑烷基酮(3-amino-2-oxazolidinone, AOZ)残留的分析方法。方法 大菱鲆冻干鱼粉样品复水后, 经盐酸水解, 2-硝基苯甲醛衍生化, 乙酸乙酯提取, 高速离心净化, 采用2 mmol/L乙酸铵(A)和甲醇(B)作为流动相进行梯度洗脱, 质谱(electron spray ionization, ESI+)选择反应监测模式对AOZ进行定性和定量测定。结果 在1.0~40 μg/L范围内线性关系良好, 相关系数大于0.999。AOZ在2.00、5.00、10.0和20.0 μg/kg添加水平的回收率在94.2%~100%之间, 批内和批间相对标准偏差均<10%。本方法冻干鱼粉中AOZ的定量限为2.00 μg/kg。结论 该方法灵敏、准确, 操作简便, 适用于大菱鲆鱼粉中AOZ残留基体标准物质的定值测定。

英文摘要:

      Objective To establish a method for the determination of furazolidone metabolite 3-amino-2-o xazolidinone (AOZ) residues in turbot fish meal by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods After rehydration, the turbot fish meal was hydrolyzed by hydrochloric acid and derivatized by 2-nitrobenzaldehyde overnight. Then AOZ was extracted with ethyl acetate and purified by high-speed centrifugation. The AOZ residue in the extract was separated on a reversed phase using a gradient elution program of 2 mmol/L ammonium acetate (A) and methanol (B). Using LC-MS/MS (ESI+) with selected reactions monitoring, identification of the major components of the AOZ residue was performed based upon the intensities of fragments. Results The calibration curve showed a good linearity in a range of 1.0?40 μg/L with the correlation coefficient over 0.999. The recoveries were ranged from 94.2% to 100% for the AOZ residues with 4 spiked levels of 2.00, 5.00, 10.0 and 20.0 μg/kg. The relative standard deviations (RSDs) were less than 10% (n=6), and the limit of quantitation (LOQ) for the AOZ in turbot fish meal was 2.00 μg/kg. Conclusion The proposed method is sensitive, accurate and easy to operate, which is suitable for detecting AOZ residues in reference material of turbot fish meal.