<p>Magnetic mixed cation exchange material (MMCX) was utilized as an efficient adsorbent in magnetic solid-phase extraction (MSPE) for the determination and identification of 30 β-agonists in animal-derived foods. This was coupled with ultrahigh performance liquid chromatography quadrupole high-field high-resolution mass spectrometry following sample pretreatment by enzymatic probe sonication (EPS) and MSPE. The purification procedures for both EPS and MSPE were appropriately optimized. Under the optimized conditions, the method demonstrated limits of detection (LODs) and quantification (LOQs) in the ranges of 0.03&#xa0;~&#xa0;0.30&#xa0;μg/kg and 0.1&#xa0;~&#xa0;1.0&#xa0;μg/kg, respectively, which are superior to those reported in existing methods. Satisfactory recoveries ranged from 84.3% to 105.8%, with relative standard deviations below 15%. Matrix effects were observed as signal suppression, ranging from 5.1% to 29.3%. The established method also exhibited good linearity with correlation coefficients (<i>r</i>) greater than 0.994. This methodology allows sample processing to be completed within 20&#xa0;min, significantly reducing both detection time and cost. The method has been validated using positive samples obtained from animals administered β-agonists and has been successfully applied to residue monitoring of β-agonists in animal-derived foods.</p>

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Determination and Identification of 30 β-Agonists in Animal-Derived Foods by Automated Magnetic Solid Phase Extraction Followed by Ultrahigh Performance Liquid Chromatography Quadrupole High Field High Resolution Mass Spectrometry Analysis

  • Decheng Suo,
  • Zhiming Xiao,
  • Ruiguo Wang,
  • Xiaoyan Pei,
  • Xiaoxu Han,
  • Hongyan Xu,
  • Shi Wang,
  • Yang Li,
  • Xia Fan

摘要

Magnetic mixed cation exchange material (MMCX) was utilized as an efficient adsorbent in magnetic solid-phase extraction (MSPE) for the determination and identification of 30 β-agonists in animal-derived foods. This was coupled with ultrahigh performance liquid chromatography quadrupole high-field high-resolution mass spectrometry following sample pretreatment by enzymatic probe sonication (EPS) and MSPE. The purification procedures for both EPS and MSPE were appropriately optimized. Under the optimized conditions, the method demonstrated limits of detection (LODs) and quantification (LOQs) in the ranges of 0.03 ~ 0.30 μg/kg and 0.1 ~ 1.0 μg/kg, respectively, which are superior to those reported in existing methods. Satisfactory recoveries ranged from 84.3% to 105.8%, with relative standard deviations below 15%. Matrix effects were observed as signal suppression, ranging from 5.1% to 29.3%. The established method also exhibited good linearity with correlation coefficients (r) greater than 0.994. This methodology allows sample processing to be completed within 20 min, significantly reducing both detection time and cost. The method has been validated using positive samples obtained from animals administered β-agonists and has been successfully applied to residue monitoring of β-agonists in animal-derived foods.