关键词: 残留, 超高效液相色谱-串联质谱, 牛肉组织, 食源性兴奋剂类药物

Abstract:

A method for the simultaneous determination of 18 food-borne stimulant drug residues in beef was developed based on ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The beef sample was extracted with acidified acetonitrile, cleaned up by Captiva filtration cartridge. The extract was dried with anhydrous magnesium sulfate, and then concentrated by nitrogen flow. The obtained residue was re-dissolved in methanol-water (7:3, v/v). The separation was performed on an Agilent Zorbax Phenyl-Hexyl column with 5 mmol/L ammonium acetate solution (containing 0.01% (v/v) acetic acid) and methanol-acetonitrile (7:3, v/v) as mobile phases with gradient elution. The analyte was detected in positive and negative ion modes and the multiple reaction monitoring (MRM) mode. The quantification analysis was performed by external standard method using matrix-matched calibration curves. The method was linear with the correlation coefficients (R²) ≥ 0.9950 in the range of 0.10-50 μg/L. At the spiked levels of 0.4, 1.0 and 2.0 μg/kg, the recoveries of all compounds ranged from 57.3% to 117.5%, with RSDs in range of 3.1%-15.6% (n=5). The limits of detection and limits of quantification were in the range of 0.0006-0.0900 μg/kg and 0.0020-0.3000 μg/kg, respectively. The method is simple, rapid, accurate and sensitive, and can meet the requirement for the determination of the 18 food-borne stimulant drug residues in beef.

Key words: beef tissue, food-borne stimulant drug, residues, ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)