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Analysis of β-agonists in different biological matrices by liquid chromatography–tandem mass spectrometry

Tomasz Śniegocki
Tomasz Śniegocki
, 
Bartosz Sell
Bartosz Sell
 and 
Andrzej Posyniak
Andrzej Posyniak
   | Nov 20, 2021
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Article Category: Review article
Published Online: Nov 20, 2021
Page range: 469 - 475
Received: Apr 19, 2021
Accepted: Oct 20, 2021
DOI: https://doi.org/10.2478/jvetres-2021-0058
Keywords
© 2021 T. Śniegocki et al. published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Fig. 1

Chromatograms of blank and spiked lung matrices with β-agonists at 0.2 μg kg−1 for clenbuterol, mabuterol, mapenterol, brombuterol, and at 1.0 μg kg−1 for salbutamol and zilpaterol, ractopamine, isoxsuprine, and terbutaline
Chromatograms of blank and spiked lung matrices with β-agonists at 0.2 μg kg−1 for clenbuterol, mabuterol, mapenterol, brombuterol, and at 1.0 μg kg−1 for salbutamol and zilpaterol, ractopamine, isoxsuprine, and terbutaline

Mass spectrometry parameters for precursor ions and product ion transitions of β-agonists and internal standards

Analyte Retention time (min) Precursor ion (m/z) Ion transition Declustering potential Collision energy (eV)
Brombuterol 4.2 366.8 213.9 56 43
292.8 47
Clenbuterol 4.1 276.8 203.0 76 23
132.1 47
Isoxsuprine 4.3 302.2 150.0 61 31
107.0 37
237.0 25
Mabuterol 4.3 310.9 217.0 20 35
237.0 25
Mapenterol 4.5 324.9 217.0 146 33
Salbutamol 3.2 239.9 148.0 131 25
166.1 19
Ractopamine 4.0 301.9 164.1 16 23
136.1 31
Terbutaline 3.2 225.9 152.1 121 23
125.1 35
Zilpaterol 3.1 261.9 185.0 26 35
202.0 27
Clebuterol-D9 4.1 285.9 204.0 31 25
Isoxsuprine -D5 4.3 307.2 150.0 61 23
Mabuterol-D9 4.3 319.9 238.0 76 25
Mapenterol-D11 4.5 335.9 238.0 76 25
Ractopamine-D6 4.0 308.0 168.1 56 23
Salbutamol-D6 3.2 248.9 148.0 136 27

Validation report for β-agonists

Matrix Repeatability (RSDr,%) Within-lab reproducibility (RSDwR,%) CCα (μg kg−1) CCβ (μg kg−1) Apparent recovery (%) Concentration range (ng/mL) Matrix effect (%) Expanded uncertainty (μg kg−1)
Clenbuterol
drinking water 4.1 ± 3.8 4.5 ± 4.0 0.10 0.11 103.9 ± 4.3 0.1–1.6 4.3 ± 3.9% 0.20 ± 0.02
feed 6.2 ± 4.6 5.6 ± 6.1 2.50 2.70 104.5 ± 6.8 2.5–40.0 5.0 ± 3.9% 5.00 ± 1.14
liver 4.3 ± 4.1 5.1 ± 4.7 0.10 0.12 103.5 ± 6.2 0.1–1.6 6.1 ± 3.2% 0.20 ± 0.06
urine 4.6 ± 3.7 5.3 ± 4.4 0.10 0.11 102.6 ± 5.1 0.1–1.6 5.6 ± 2.7% 0.20 ± 0.04
muscle 5.9 ± 6.5 4.5 ± 7.6 0.05 0.06 109.1 ± 4.4 0.1–1.6 4.3 ± 6.5% 0.10 ± 0.02
lung 4.3 ± 3.8 4.8 ± 4.6 0.10 0.11 96.1 ± 4.9 0.1–1.6 5.3 ± 4.9% 0.20 ± 0.05
Mabuterol
drinking water 3.7 ± 3.6 4.7 ± 3.9 0.10 0.11 99.5 ± 4.8 0.1–1.6 4.0 ± 3.5% 0.20 ± 0.03
feed 5.6 ± 5.4 6.7 ± 5.6 2.50 2.62 106.2 ± 7.8 2.5–40.0 6.0 ± 3.3% 5.00 ± 1.25
liver 5.9 ± 5.8 7.3 ± 6.3 0.10 0.12 95.4 ± 7.3 0.1–1.6 6.3 ± 5.2% 0.20 ± 0.05
urine 5.2 ± 4.9 6.3 ± 5.1 0.10 0.11 103.0 ± 4.1 0.1–1.6 5.4 ± 4.9% 0.20 ± 0.04
muscle 6.3 ± 4.1 6.4 ± 5.0 0.05 0.06 95.9 ± 6.0 0.05–0.8 5.8 ± 5.0% 0.10 ± 0.02
lung 5.9 ± 3.9 6.6 ± 5.6 0.10 0.11 93.2 ± 4.6 0.1–1.6 6.3 ± 4.6% 0.20 ± 0.04
Mapenterol
drinking water 3.2 ± 3.4 4.1 ± 4.0 0.10 0.12 98.9 ± 4.8 0.1–1.6 4.0 ± 2.0% 0.10 ± 0.02
feed 5.4 ± 4.6 5.6 ± 7.1 2.50 2.61 105.1 ± 5.6 2.5–40.0 5.1 ± 2.9% 5.00 ± 1.14
liver 5.4 ± 5.0 6.4 ± 5.2 0.10 0.12 93.3 ± 5.6 0.1–1.6 5.4 ± 4.9% 0.20 ± 0.04
urine 5.3 ± 4.5 5.4 ± 4.9 0.20 0.12 102.0 ± 5.5 0.1–1.6 4.9 ± 5.1% 0.20 ± 0.04
muscle 4.1 ± 3.4 5.0 ± 4.2 0.05 0.06 97.0 ± 5.3 0.05–0.8 5.5 ± 4.1% 0.10 ± 0.02
lung 3.9 ± 3.7 5.4 ± 4.8 0.10 0.11 100.3 ± 6.1 0.1–1.6 4.8 ± 5.2% 0.20 ± 0.05
Brombuterol
drinking water 3.1 ± 3.3 4.2 ± 4.1 0.10 0.12 95.4 ± 4.3 0.1–1.6 4.0 ± 3.6% 0.20 ± 0.05
feed 5.6 ± 4.1 6.2 ± 4.0 2.50 2.67 103.2 ± 6.8 2.5–40.0 5.3 ± 3.9% 5.00 ± 1.24
liver 4.9 ± 4.7 5.3 ± 4.9 0.10 0.11 96.5 ± 6.8 0.1–1.6 6.1 ± 4.8% 0.20 ± 0.05
urine 4.5 ± 3.9 5.1 ± 4.1 0.10 0.11 99.6 ± 5.2 0.1–1.6 5.1 ± 4.6% 0.20 ± 0.04
muscle 4.6 ± 4.7 5.4 ± 4.8 0.05 0.06 105.4 ± 5.4 0.05–0.8 4.5 ± 5.3% 0.10 ± 0.03
lung 4.9 ± 3.5 5.4 ± 4.6 0.10 0.12 98.2 ± 4.9 0.1–1.6 5.3 ± 3.6% 0.20 ± 0.05
Ractopamine
drinking water 3.1 ± 3.7 4.6 ± 3.6 0.50 0.57 103.5 ± 3.9 0.5–8.0 3.9 ± 4.1% 1.00 ± 0.23
feed 4.4 ± 3.1 5.6 ± 4.6 2.50 2.56 102.3 ± 5.2 2.5–40.0 6.0 ± 3.2% 5.00 ± 1.35
liver 4.0 ± 4.3 4.6 ± 4.9 0.50 0.52 103.6 ± 6.8 0.5–8.0 5.3 ± 6.0% 1.00 ± 0.26
urine 4.2 ± 3.8 5.3 ± 4.2 0.50 0.52 102.8 ± 5.1 0.5–8.0 5.8 ± 5.3% 1.00 ± 0.23
muscle 4.6 ± 4.9 5.4 ± 5.3 0.50 0.52 105.0 ± 4.7 0.5–8.0 6.5 ± 5.7% 1.00 ± 0.16
lung 4.9 ± 4.5 5.4 ± 4.9 0.50 0.56 103.8 ± 4.3 0.5–8.0 5.5 ± 3.9% 1.00 ± 0.26
Salbutamol
drinking water 4.2 ± 2.4 5.4 ± 4.0 2.50 2.54 104.9 ± 4.8 2.5–40.0 5.3 ± 3.1% 5.00 ± 1.25
feed 5.9 ± 4.6 6.5 ± 6.6 2.50 2.72 105.1 ± 6.9 2.5–40.0 6.0 ± 4.1% 5.00 ± 1.31
liver 5.3 ± 4.7 7.4 ± 5.2 2.50 2.61 93.3 ± 5.6 2.5–40.0 6.5 ± 5.4% 5.00 ± 1.45
urine 4.9 ± 4.8 6.4 ± 4.9 0.50 0.52 97.0 ± 6.3 0.5–8.0 5.4 ± 5.5% 1.00 ± 0.25
muscle 5.2 ± 3.3 5.7 ± 4.3 2.50 2.61 105.3 ± 4.6 2.5–40.0 6.5 ± 6.5% 5.00 ± 1.16
lung 4.9 ± 4.5 5.0 ± 4.6 0.50 0.52 101.5 ± 5.1 0.5–8.0 4.8 ± 5.6% 1.00 ± 0.33
Zilpaterol
drinking water 3.2 ± 2.4 4.1 ± 3.0 2.50 2.58 105.4 ± 4.8 2.5–40.0 3.0 ± 2.1% 5.00 ± 1.19
feed 4.1 ± 4.5 5.9 ± 4.6 2.50 2.73 104.5 ± 6.3 2.5–40.0 5.3 ± 3.9% 5.00 ± 1.40
liver 6.4 ± 5.7 7.7 ± 6.2 2.50 2.79 107.3 ± 5.6 2.5–40.0 6.3 ± 6.3% 5.00 ± 1.52
urine 7.1 ± 4.3 8.0 ± 4.9 0.50 0.56 100.3 ± 6.8 0.5–8.0 5.3 ± 4.6% 1.00 ± 0.23
muscle 5.1 ± 4.3 5.9 ± 4.8 2.50 2.69 112.0 ± 6.1 2.5–40.0 7.3 ± 5.5% 5.00 ± 1.64
lung 4.0 ± 3.5 8.2 ± 7.6 0.50 0.56 106.4 ± 5.3 0.5–8.0 7.0 ± 4.3% 1.00 ± 0.45
Terbutaline
drinking water 5.2 ± 4.4 6.0 ± 4.5 5.00 5.34 106.9 ± 3.8 5.0–80.0 5.1 ± 4.6% 10.00 ± 3.60
feed 6.2 ± 3.6 7.6 ± 3.9 2.50 2.70 107.5 ± 7.1 2.5–40.0 6.6 ± 4.3% 5.00 ± 1.72
liver 4.2 ± 4.7 6.1 ± 5.7 5.00 5.25 93.3 ± 5.1 5.0–80.0 5.7 ± 6.1% 10.00 ± 3.12
urine 6.1 ± 4.2 7.3 ± 5.0 1.50 1.54 102.0 ± 6.5 1.5–24.0 8.8 ± 4.7% 3.00 ± 0.86
muscle 3.4 ± 3.2 4.2 ± 3.6 5.00 5.63 105.3 ± 3.8 5.0–80.0 3.5 ± 3.5% 10.00 ± 4.1
lung 5.2 ± 3.5 6.0 ± 4.0 1.50 1.64 96.3 ± 5.1 1.5–24.0 6.3 ± 6.2% 3.00 ± 0.82
Isoxsuprine
drinking water 3.6 ± 4.3 4.4 ± 5.1 0.25 0.27 102.9 ± 4.9 0.25–4.0 3.2 ± 2.3% 0.50 ± 0.09
feed 3.6 ± 3.7 4.6 ± 4.0 2.50 2.59 104.5 ± 2.8 2.5–40.0 5.0 ± 4.9% 5.00 ± 1.19
liver 3.8 ± 4.0 4.9 ± 5.2 0.25 0.26 102.3 ± 4.3 0.25–4.0 4.6 ± 4.5% 0.50 ± 0.11
urine 4.9 ± 3.8 5.4 ± 4.5 0.25 0.26 106.2 ± 4.6 0.25–4.0 5.3 ± 4.0% 0.50 ± 0.12
muscle 3.6 ± 3.8 4.3 ± 4.1 0.25 0.26 98.0 ± 4.3 0.25–4.0 4.5 ± 3.5% 0.50 ± 0.08
lung 3.6 ± 4.5 5.8 ± 5.6 0.25 0.27 108.0 ± 6.2 0.25–4.0 4.3 ± 5.0% 0.50 ± 0.12

Concentration levels used for validation of the β-agonist detection method in different matrices

Analyte drinking water μg kg−1 feed μg kg−1 liver μg kg−1 urine μg kg−1 muscle μg kg−1 lung μg kg−1
Brombuterol 0.1; 0.2; 0.4; 1.6 2.5; 5.0; 10.0; 40.0 0.1; 0.2; 0.4; 1.6 0.1; 0.2; 0.4; 1.6 0.05; 0.1; 0.2; 0.8 0.1; 0.2; 0.4; 1.6
Clenbuterol 0.1; 0.2; 0.4; 1.6 2.5; 5.0; 10.0; 40.0 0.1; 0.2; 0.4; 1.6 0.1; 0.2; 0.4; 1.6 0.05; 0.1; 0.2; 0.8 0.1; 0.2; 0.4; 1.6
Isoxsuprine 0.25; 0.5; 1.0; 4.0 2.5; 5.0; 10.0; 40.0 0.25; 0.5; 1.0; 4.0 0.25; 0.5; 1.0; 4.0 0.25; 0.5; 1.0; 4.0 0.25; 0.5; 1.0; 4.0
Mabuterol 0.1; 0.2; 0.4; 1.6 2.5; 5.0; 10.0; 40.0 0.1; 0.2; 0.4; 1.6 0.1; 0.2; 0.4; 1.6 0.05; 0.1; 0.2; 0.8 0.1; 0.2; 0.4; 1.6
Mapenterol 0.1; 0.2; 0.4; 1.6 2.5; 5.0; 10.0; 40.0 0.1; 0.2; 0.4; 1.6 0.1; 0.2; 0.4; 1.6 0.05; 0.1; 0.2; 0.8 0.1; 0.2; 0.4; 1.6
Salbutamol 2.5; 5.0; 10.0; 40.0 2.5; 5.0; 10.0; 40.0 2.5; 5.0; 10.0; 40.0 0.5; 1.0; 2.0; 8.0 2.5; 5.0; 10.0; 40.0 0.5; 1.0; 2.0; 8.0
Ractopamine 0.5; 1.0; 2.0; 8.0 2.5; 5.0; 10.0; 40.0 0.5; 1.0; 2.0; 8.0 0.5; 1.0; 2.0; 8.0 0.5; 1.0; 2.0; 8.0 0.5; 1.0; 2.0; 8.0
Terbutaline 5.0; 10.0; 20.0; 80.0 2.5; 5.0; 10.0; 40.0 5.0; 10.0; 20.0; 80.0 1.5; 3.0; 6.0; 24.0 5.0; 10.0; 20.0; 80.0 1.5; 3.0; 6.0; 24.0
Zilpaterol 2.5; 5.0; 10.0; 40.0 2.5; 5.0; 10.0; 40.0 2.5; 5.0; 10.0; 40.0 0.5; 1.0; 2.0; 8.0 2.5; 5.0; 10.0; 40.0 0.5; 1.0; 2.0; 8.0
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