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Development of a method for the determination of sedatives in bovine and porcine urine and kidneys by liquid chromatography–tandem mass spectrometry

Tomasz Śniegocki
Tomasz Śniegocki
, 
Elżbieta Samorek
Elżbieta Samorek
, 
Bartosz Sell
Bartosz Sell
 y 
Weronika Krajewska
Weronika Krajewska
   | 23 mar 2024
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Publicado en línea: 23 mar 2024
Páginas: 137 - 145
Recibido: 17 ago 2023
Aceptado: 04 ene 2024
DOI: https://doi.org/10.2478/jvetres-2024-0001
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© 2024 Tomasz 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 kidney samples. A) carazolol; B) acepromazine; C) azaperol; D) azaperone; E) haloperidol; F) chlorpromazine; G) xylazine; H) propionylpromazine
Chromatograms of blank kidney samples. A) carazolol; B) acepromazine; C) azaperol; D) azaperone; E) haloperidol; F) chlorpromazine; G) xylazine; H) propionylpromazine

Fig. 2.

Chromatograms of kidney tissue samples spiked at 5.0 μg kg−1 for A) carazolol (tR = 2.61); B) acepromazine (tR = 2.76); C) azaperol (tR = 2.61); D) azaperone (tR = 2.66); E) haloperidol (tR = 2.73); F) chlorpromazine (tR = 2.85); G) xylazine (tR = 2.52); H) propionylpromazine (tR = 2.81)
Chromatograms of kidney tissue samples spiked at 5.0 μg kg−1 for A) carazolol (tR = 2.61); B) acepromazine (tR = 2.76); C) azaperol (tR = 2.61); D) azaperone (tR = 2.66); E) haloperidol (tR = 2.73); F) chlorpromazine (tR = 2.85); G) xylazine (tR = 2.52); H) propionylpromazine (tR = 2.81)

Fig. 3.

Matrix effect in liquid chromatography–tandem mass spectrometry to detect sedatives in pig and cattle kidney tissue and urine. APN – azaperone; APL – azaperol; CAR – carazolol; ClPN – chlorpromazine; AcPN – acepromazine; HPL – haloperidol; PrPN – propionylpromazine; XyN – xylazine. Red lines – boundaries of suppressive (lower) or enhancing (upper) matrix effect
Matrix effect in liquid chromatography–tandem mass spectrometry to detect sedatives in pig and cattle kidney tissue and urine. APN – azaperone; APL – azaperol; CAR – carazolol; ClPN – chlorpromazine; AcPN – acepromazine; HPL – haloperidol; PrPN – propionylpromazine; XyN – xylazine. Red lines – boundaries of suppressive (lower) or enhancing (upper) matrix effect

Fig. 4.

Comparison of extracted dry mass (g) from 1 g kidney samples using different methods. Method 1 – standard method; Method 2 – standard method with modification (nylon filter); Method 3 – standard method with modification (TiO2); Method 4 – standard method with modification (ethyl acetate)
Comparison of extracted dry mass (g) from 1 g kidney samples using different methods. Method 1 – standard method; Method 2 – standard method with modification (nylon filter); Method 3 – standard method with modification (TiO2); Method 4 – standard method with modification (ethyl acetate)

Fig. 5.

Chromatograms of glycerophosphocholines (184 m/z) and 2-lyso-glycerophosphocholines (104 m/z) (A) after acetonitrile extraction, (B) after ethyl acetate extraction from kidney
Chromatograms of glycerophosphocholines (184 m/z) and 2-lyso-glycerophosphocholines (104 m/z) (A) after acetonitrile extraction, (B) after ethyl acetate extraction from kidney

Validation results for determination of neuroleptics in kidney and urine

Analyte Matrix Repeatability (RSDr, %) Within-lab reproducibility (RSDwR, %) Apparent recovery (%) Expanded uncertainty (μg kg−1) CCα (μg kg−1)
Acepromazine Kidney 9.3 7.1 97.1 0.82 2.5
Urine 9.8 8.3 101.6 1.04 2.5
Azaperol Kidney 9.5 6.7 100.6 0.85 2.5
Urine 7.7 8.1 101.0 1.10 2.5
Azaperone Kidney 7.0 5.5 100.5 0.80 2.5
Urine 6.0 5.2 101.2 0.67 2.5
Carazolol Kidney 6.4 5.0 99.9 0.70 2.5
Urine 7.4 9.8 101.6 1.43 2.5
Chlorpromazine Kidney 7.4 9.2 100.5 1.43 2.5
Urine 6.6 7.3 101.3 0.96 2.5
Haloperidol Kidney 8.0 10.4 97.2 1.49 2.5
Urine 12.0 18.0 100.6 2.03 2.5
Propionylpromazine Kidney 8.5 8.3 97.3 1.08 2.5
Urine 9.5 8.2 102.1 1.28 2.5
Xylazine Kidney 9.2 10.5 99.3 1.45 2.5
Urine 9.4 8.7 100.0 1.13 2.5

Mass spectrometry parameters for precursor ions and product ion transitions of neuroleptics and internal standards

Analyte Retention time (min) Precursor ion (m/z) Ion transition (m/z) Declustering potential (eV) Collision energy (eV)
Acepromazine 2.76 326.9 86.1 100 24
58.2 72
Azaperol 2.61 330.1 121.0 96 29
312.0 21
Azaperone 2.65 328.1 165.0 91 27
122.9 43
Carazolol 2.60 299.1 116.0 96 27
222.0 27
Chlorpromazine 2.85 319.0 86.0 96 25
245.9 31
Haloperidol 2.74 376.0 165.1 110 30
123.0 43
Propionylpromazine 2.82 341.0 58.0 95 70
86.0 25
Xylazine 2.52 221.0 90.0 100 27
164.1 33
Acepromazine - D6 2.76 333.0 92.0 110 25
64.0 69
Azaperol - D4 2.61 334.1 121.0 96 31
153.0 39
Azaperone - D4 2.65 332.1 169.0 101 29
121.0 29
Carazolol - D7 2.60 306.1 123.1 101 27
222.0 27
Chlorpromazine - D6 2.85 325.0 92.1 81 25
245.9 33
Propionylpromazine - D6 2.82 347.0 92.1 100 24
64.1 70
Xylazine - D6 2.52 226.9 90.0 120 29
170.0 34
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