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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 Cover

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

Journal of Veterinary Research
Volume 68 (2024): Issue 1 (March 2024)
By: Tomasz Śniegocki,  Elżbieta Samorek,  Bartosz Sell and  Weronika Krajewska  
Open Access
|Mar 2024

Figures & Tables

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

AnalyteMatrixRepeatability (RSDr, %)Within-lab reproducibility (RSDwR, %)Apparent recovery (%)Expanded uncertainty (μg kg−1)CCα (μg kg−1)
AcepromazineKidney9.37.197.10.822.5
Urine9.88.3101.61.042.5
AzaperolKidney9.56.7100.60.852.5
Urine7.78.1101.01.102.5
AzaperoneKidney7.05.5100.50.802.5
Urine6.05.2101.20.672.5
CarazololKidney6.45.099.90.702.5
Urine7.49.8101.61.432.5
ChlorpromazineKidney7.49.2100.51.432.5
Urine6.67.3101.30.962.5
HaloperidolKidney8.010.497.21.492.5
Urine12.018.0100.62.032.5
PropionylpromazineKidney8.58.397.31.082.5
Urine9.58.2102.11.282.5
XylazineKidney9.210.599.31.452.5
Urine9.48.7100.01.132.5

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

AnalyteRetention time (min)Precursor ion (m/z)Ion transition (m/z)Declustering potential (eV)Collision energy (eV)
Acepromazine2.76326.986.110024
58.272
Azaperol2.61330.1121.09629
312.021
Azaperone2.65328.1165.09127
122.943
Carazolol2.60299.1116.09627
222.027
Chlorpromazine2.85319.086.09625
245.931
Haloperidol2.74376.0165.111030
123.043
Propionylpromazine2.82341.058.09570
86.025
Xylazine2.52221.090.010027
164.133
Acepromazine - D62.76333.092.011025
64.069
Azaperol - D42.61334.1121.09631
153.039
Azaperone - D42.65332.1169.010129
121.029
Carazolol - D72.60306.1123.110127
222.027
Chlorpromazine - D62.85325.092.18125
245.933
Propionylpromazine - D62.82347.092.110024
64.170
Xylazine - D62.52226.990.012029
170.034
DOI: https://doi.org/10.2478/jvetres-2024-0001 | Journal eISSN: 2450-8608
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Language: English
Page range: 137 - 145
Submitted on: Aug 17, 2023
Accepted on: Jan 4, 2024
Published on: Mar 23, 2024
Published by: National Veterinary Research Institute in Pulawy
In partnership with: Paradigm Publishing Services
Publication frequency: 4 issues per year
Keywords:
sedatives,
tranquillisers,
QuEChERS,
liquid chromatography–tandem mass spectrometry,
Commission Implementing Regulation (EU) 2021/808
Related subjects:
Life sciences,
Molecular biology,
Microbiology and virology,
Life sciences, other,
Medicine,
Veterinary medicine

© 2024 Tomasz Śniegocki, Elżbieta Samorek, Bartosz Sell, Weronika Krajewska, published by National Veterinary Research Institute in Pulawy
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

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