液相色谱-串联质谱法同时检测饲料和牛血清中吡喹酮药物残留

Simultaneous determination of praziquantel residues in feed and bovine serum by liquid chromatography-tandem mass spectrometry

中文关键词:  吡喹酮  液相色谱-串联质谱法  饲料  牛血清  残留

英文关键词:praziquantelt  liquid chromatography-tandem mass spectrometry  feed  bovine serum  residues

中文摘要:

      目的 建立一种用液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)检测饲料和牛血清中吡喹酮药物残留的方法。方法 样品经乙腈/水提取液提取,过固相萃取柱净化。采用0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱, 采用多离子检测模式对吡喹酮药物的定量离子和定性离子进行监测。结果 8 min内完成目标化合物的分离分析。吡喹酮在0.05、0.1和0.5 ng/mL添加水平的回收率为75.0%~99.0%, 相对标准偏差小于5.4%(n=6)。结论 该方法快速、准确、灵敏, 适合测定食用活动物体内的吡喹酮药物残留。

英文摘要:

      Objective To establish a method for the determination of praziquantel residues in feed and bovine serum by liquid chromatography-tandem mass spectrometric (LC–MS/MS). Methods Samples were extracted with acetonitrile and ultrapure water, and then purified by solid-phase extraction column. The praziquantel residues in the extracts were separated on a reversed phase column using a gradient elution program of 0.1% formic acid aqueous solution and acetonitrile. Using LC–MS/MS with multiple reactions monitoring (MRM), identification of the praziquantel residues was performed based upon the intensities of fragments. Results Separation and analysis of target compounds could achieved within 8 min. The recoveries were 75.0%~99.0% for praziquantel residues with 3 spiked levels of 0.05, 0.1 and 0.5 ng/mL. The relative standard deviations (RSD) were less than 5.4% (n=6). Conclusion The proposed method is fast, accurate and sensitive, which is suitable for detecting praziquantel residues in food and feed samples.