超高效液相色谱-串联质谱法测定猪肉、猪肝及猪尿中的阿托品残留

Determination of Atropine in Porcine Muscle,Liver and Urine by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

关键词:  猪组织  猪尿  阿托品  残留  超高效液相色谱-串联质谱

Key words:  porcine tissues  porcine urine  atropine  residue  UPLC-MS/MS

摘要:

建立了猪肉、猪肝和猪尿中阿托品残留的超高效液相色谱-串联质谱(UPLC-MS/MS)的检测方法。样品经乙腈-0.1%甲酸水(V/V,90:10)溶液提取,Agela Cleanert? PEP-2固相萃取柱净化后,采用UPLC-MS/MS测定,外标法定量。结果表明,猪组织及猪尿中阿托品的检测限为0.2 μg/kg,定量限为0.5 μg/kg。在0.5～2.5 μg/kg添加浓度范围内阿托品的平均回收率78.3%～98.2%之间,批内、批间相对标准偏差均小于15％。该方法简便、快速、灵敏度高、重现性好,适用于猪组织及猪尿中阿托品的含量测定。

Abstract:

A method based on ultra performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was developed for determination of atropine in porcine muscle,liver and urine. The analyte was extracted with acetonitrile-0.1% formic acid in water (V/V,90:10),and was cleaned up by the Agela Cleanert? PEP-2cartridge. Quantification of the analyte was achieved by UPLC-MS/MS with multiple reaction monitoring (MRM) using external standard method. The results indicated that the detection limits and quantification limits of the method were 0.2 μg/kg and 0.5 μg/kg. The average recoveries of the drugs ranged from 78.3%～98.2% at spiked levels of 0.5~2.5 μg/kg with RSD less than 15%. The method was convenient,rapid,sensitive and reproducibility for monitoring atropine residues in porcine muscle,liver and urine。