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Determination of steroid esters in hair of slaughter animals by liquid chromatography with tandem mass spectrometry

Iwona Matraszek-Żuchowska

Iwona Matraszek-Żuchowska

Department of Pharmacology and Toxicology, National Veterinary Research InstitutePuławy, Poland
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Matraszek-Żuchowska, Iwona
, 
Barbara Woźniak

Barbara Woźniak

Department of Pharmacology and Toxicology, National Veterinary Research InstitutePuławy, Poland
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Woźniak, Barbara
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Katarzyna Sielska

Katarzyna Sielska

Department of Pharmacology and Toxicology, National Veterinary Research InstitutePuławy, Poland
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Sielska, Katarzyna
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Andrzej Posyniak

Andrzej Posyniak

Department of Pharmacology and Toxicology, National Veterinary Research InstitutePuławy, Poland
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Posyniak, Andrzej
  
08 ott 2019
Determination of steroid esters in hair of slaughter animals by liquid chromatography with tandem mass spectrometry's Cover Image
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Pubblicato online: 08 ott 2019
Pagine: 561 - 572
Ricevuto: 08 feb 2019
Accettato: 16 set 2019
DOI: https://doi.org/10.2478/jvetres-2019-0061
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© 2019 I. Matraszek-Żuchowska et al. published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Fig. 1

Structural formulas of molecules of steroid esters
Structural formulas of molecules of steroid esters

Fig. 2

LC–MS/MS MRM chromatograms of steroid esters (testosterone propionate, nortestosterone phenylpropionate, testosterone benzoate, boldenone undecylenate, and nortestosterone decanoate) in bovine hair samples spiked at 10 μg kg−1
LC–MS/MS MRM chromatograms of steroid esters (testosterone propionate, nortestosterone phenylpropionate, testosterone benzoate, boldenone undecylenate, and nortestosterone decanoate) in bovine hair samples spiked at 10 μg kg−1

Fig. 3

LC–MS/MS MRM chromatograms of steroid esters in a blank bovine hair sample in which no testosterone propionate, nortestosterone phenylpropionate, testosterone benzoate, boldenone undecylenate, or nortestosterone decanoate were found in official monitoring studies
LC–MS/MS MRM chromatograms of steroid esters in a blank bovine hair sample in which no testosterone propionate, nortestosterone phenylpropionate, testosterone benzoate, boldenone undecylenate, or nortestosterone decanoate were found in official monitoring studies

Parameters of analytical efficiency of the LC-MS/MS method for the determination of steroid esters in animal hair

Compound TP TB BU NTD NTPhP
Apparent recovery 5*
 96.4 104.7 93.1 96.0 109.7
(%) 10
 84.3 108.5 92.7 98.1 89.7
15
 92.3 96.5 89.1 95.8 92.6
20
 97.3 107.2 102.5 109.3 103.8
50
 93.4 91.8 90.1 97.9 88.8
CCα
 90.4 92.0 95.7 92.1 89.8
Repeatability 5
 11.8 14.6 10.1 25.4 8.6
(RSD, %) 10
 19.7 12.7 20.4 11.2 21.7
15
 26.1 9.2 17.9 19.0 29.6
CCα
 11.8 10.5 11.3 13.6 12.9
Within-lab 5
 29.9 39.8 39.9 32.1 17.4
reproducibility 10
 22.6 13.9 26.7 17.6 21.7
(RSD, %) 15 37.2 34.4 39.7 30.6 37.0
Decision (CCα, μg limit kg−1) 3.51 2.57 3.51 3.98 4.18
Detection (CCβ, μg capability kg−1) 5.98 4.38 5.99 6.78 7.12
Measurement uncertainty at validation level of 10 μg kg−1 (U, k = 2, %) 38.0 30.2 49.4 37.8 39.0
Matrix effect (%) −5.2 −23.6 22.3 −16.9 −18.2
Comparison of accuracy and repeatability in bovine (n = 10) and pig (n = 10) hair samples spiked at 10 μg kg−1
Apparent recovery (%) 95.2 109.2 84.6 101.2 82.5
Repeatability (RSD, %) 19.6 14.1 22.6 13.1 16.9
t testexp. 1.358 1.448 0.947 0.368 1.239
F testexp. 1.915 0.925 0.487 2.721 2.787
Standard curve Slope ± sb 0.0116 ± 0.0001 0.0245 ± 0.0032 0.2404 ± 0.0103 0.0171 ± 0.0038 0.0308 ± 0.0005
y-Intercept ± sa −0.0009 ± 0.0021 0.0408 ± 0.0182 −0.1264 ± 0.2725 −0.0073 ± 0.0173 0.0059 ± 0.0301
Correlation coefficient 0.9996 0.9983 0.9965 0.9873 0.9990
Standard error 0.0062 0.0264 0.3919 0.0536 0.0255
Matrix matched calibration
curve
Slope ± sb 0.0110 ± 0.0004 −0.0080 ± 0.0236 0.0187 ± 0.0020 0.0693 ± 0.1065 0.2939 ± 0.1603 −0.1453 ± 1.1592 0.0142 ± 0.0327 0.0728 ± 0.6266 0.0252 ± 0.0048 0.0642 ± 0.0682
sa y–Intercept ± 0.9961 0.9943 0.9928 0.9812 0.9812
Correlation coefficient Standard error 0.0187 0.0389 0.6812 0.0536 0.0947

LC–MS/MS ion acquisition parameters (MRM mode) used for the identification and confirmation of the steroid esters

MRM Collision Declustering Entrance Collision cell exit Ion ratio Samples the confirmation fulfilling criteria (%)
Compound transition (m/z) energy CE (eV) potential DP (V) potential EP (V) potential CXP (eV) average ± SD 5.0–50.0 μg kg−1 CCα level
TP 345.4 > 97.1* 29 27 - - -
345.4 > 109.3 46 4 0.608 ± 0.113 99.2 100.0
345.4 > 253.4 25 200 11 24 0.272 ± 0.073 100.0 98.1
345.4 > 271.2 25 20 0.322 ± 0.088 98.1 98.1
TB 393.3 > 97.0 42 20 0.435 ± 0.070 98.8 94.5
393.3 > 105.1 20 70 12 14 - - -
BU 453.4 > 121.3 44 10 0.466 ± 0.065 97.9 98.1
453.4 > 135.1 26 16 - - -
453.4 > 149.2 24 100 10 17 0.414 ± 0.071 95.3 92.0
453.4 > 269.1 14 21 0.814 ± 0.097 100.0 100.0
NTD 429.4 > 95.2 30 12 0.569 ± 0.114 99.1 98.0
429.4 > 155.1 26 27 - - -
429.4 > 239.0 32 180 12 18 0.319 ± 0.063 97.3 94.1
429.4 > 257.1 24 11 0.833 ± 0.095 99.2 97.8
NTPhP 407.4 > 105.0 16 - - -
407.4 > 133.0 48 200 14 23 0.266 ± 0.073 97.2 92.5
407.4 > 257.2 28 0.301 ± 0.070 98.8 98.2
T-d3P 348.4 > 97.0 28 90 11 15 - - -
T-d3B 396.4 > 105.0 28 100 10 15 - - -
T-d3D 446.4 > 97.0 51 145 10 22 - - -
Lingua:
Inglese
Frequenza di pubblicazione:
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Argomenti della rivista:
Scienze biologiche, Biologia molecolare, Microbiologia e virologia, Scienze della vita, altro, Medicina, Medicina veterinaria
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