Accès libre

Simultaneous determination of pyrrolizidine and tropane alkaloids in honey by liquid chromatography–mass spectrometry

Ewelina Kowalczyk
Ewelina Kowalczyk
 et 
Krzysztof Kwiatek
Krzysztof Kwiatek
   | 05 juil. 2022
Journal of Veterinary Research's Cover Image
À propos de cet article
Article précédent
Article suivant
Citez
Publié en ligne: 05 juil. 2022
Pages: 235 - 243
Reçu: 13 janv. 2022
Accepté: 20 juin 2022
DOI: https://doi.org/10.2478/jvetres-2022-0032
Mots clés
© 2022 E. Kowalczyk, K. Kwiatek., published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Fig. 1

Results of honey sample alkaloid investigation expressed as percentage of samples contaminated and not contaminated and percentage distribution of determined alkaloids in the contaminated samples
Results of honey sample alkaloid investigation expressed as percentage of samples contaminated and not contaminated and percentage distribution of determined alkaloids in the contaminated samples

Fig. 2

Boxplots of the concentration of determined alkaloids
Boxplots of the concentration of determined alkaloids

Fig. 3

a) SIM chromatogram obtained for honey matrix spiked at a concentration of 5 μg kg−1. 1 – monocrotaline, 2 – erucifoline, 3 – intermedine, 4 – europine, 5 – lycopsamine, 6 – jacobine, 7 – scopolamine, 8 – retrorsine, 9 – trichodesmine, 10 – heliotrine, 11 – seneciphylline, 12 – atropine, 13 – senecivernine, 14 – senecionine, 15 – echimidine, 16 – senkirkine, 17 – lasiocarpine; b) chromatogram of a blank honey sample
a) SIM chromatogram obtained for honey matrix spiked at a concentration of 5 μg kg−1. 1 – monocrotaline, 2 – erucifoline, 3 – intermedine, 4 – europine, 5 – lycopsamine, 6 – jacobine, 7 – scopolamine, 8 – retrorsine, 9 – trichodesmine, 10 – heliotrine, 11 – seneciphylline, 12 – atropine, 13 – senecivernine, 14 – senecionine, 15 – echimidine, 16 – senkirkine, 17 – lasiocarpine; b) chromatogram of a blank honey sample

Alkaloid contamination results for the honey samples tested

Intermedine Lycopsamine Senecionine Senecivernine Echimidine Retrorsine Seneciphylline Erucifoline Total
02/p 3.0 1.9 6.9 11.8
03/p 2.2 2.8 2.2 7.3 14.5
06/f 23.3 22.5 101.2 147.0
07/p 2.2 3.2 1.9 7.3
09/f 2.9 10.2 13.1
10/p 3.0 2.1 4.1 9.2
11/f 1.8 4.0 5.8
14/f 120.0 120.0
15/p 5.9 5.9
16/p 9.2 14.1 2.0 6.3 31.6
19/f 2.7 3.0 4.3 4.5 14.5
22/p 7.1 5.3 4.3 16.7
25/p 8.7 8.7
27/p 2.2 2.2
28/p 2.5 2.5

Monitored ions (m/z), retention time, matrix effect, determination coefficient (R2), limit of detection (LOD) and limit of quantification (LOQ) of analysed pyrrolizidine and tropane alkaloids

Monitored ion (m/z) Retention time (min) Matrix effect (%) Linearity R2 LOD μg kg−1 LOQ μg kg−1 Uncertainty (%)
Monocrotaline 326.1 5.26 101 0.9924 0.16 0.52 9.8
Erucifoline 350.1 7.60 95 0.9933 0.10 0.35 12.9
Intermedine 300.1 8.14 115 0.9900 0.09 0.31 19.0
Europine 330.1 8.37 115 0.9929 0.17 0.58 24.3
Lycopsamine 300.1 8.54 116 0.9877 0.09 0.28 22.1
Jacobine 352.1 9.07 94 0.9922 0.13 0.44 17.6
Retrorsine 352.1 11.49 97 0.9904 0.09 0.29 21.4
Trichodesmine 354.1 11.65 101 0.9945 0.13 0.44 13.7
Heliotrine 314.1 12.19 119 0.9952 0.11 0.37 17.7
Seneciphylline 334.1 12.79 96 0.9944 0.10 0.34 13.7
Senecivernine 336.1 15.47 98 0.9940 0.13 0.43 14.2
Senecionine 336.1 15.73 91 0.9901 0.09 0.29 17.1
Echimidine 398.1 17.25 103 0.9941 0.16 0.53 25.5
Senkirkine 366.1 17.44 113 0.9939 0.05 0.17 5.6
Lasiocarpine 412.1 18.89 115 0.9935 0.06 0.21 13.4
Scopolamine 304.1 10.28 105 0.9922 0.15 0.49 15.5
Atropine 290.1 14.36 127 0.9942 0.11 0.36 14.7

Validation results for recovery, repeatability and within-laboratory reproducibility

Recovery (%) Repeatability CV (%) Reproducibility CV (%)
Concentration 5 50 200 5 50 200 5 50 200
Monocrotaline 92.6 96.5 91.2 5.7 3.8 4.6 7.9 8.6 7.6
Erucifoline 90.6 96.9 94.9 5.4 4.1 8.0 8.6 6.2 7.9
Intermedine 100.2 98.2 88.6 5.2 9.6 13.3 7.8 9.8 12.6
Europine 98.6 95.9 81.2 3.9 11.4 12.9 8.5 11.1 17.4
Lycopsamine 97.1 95.6 84.5 4.7 11.6 12.4 9.5 11.8 15.4
Jacobine 94.0 100.6 92.1 3.3 4.5 10.0 8.0 6.7 9.6
Retrorsine 83.9 97.7 92.1 7.2 12.7 11.0 17.8 13.9 12.8
Trichodesmine 94.7 97.2 89.4 9.0 5.0 7.3 11.9 7.5 8.8
Heliotrine 99.9 100.3 92.8 7.4 5.7 9.7 6.7 7.5 9.8
Seneciphylline 90.3 99.4 95.5 7.7 3.5 8.2 9.9 8.0 8.1
Senecivernine 100.0 104.0 96.1 3.5 2.7 8.3 5.7 6.5 8.8
Senecionine 96.2 100.1 90.9 1.7 7.0 8.9 7.8 8.2 11.1
Echimidine 98.9 99.6 89.0 6.5 9.1 13.3 8.3 9.8 16.4
Senkirkine 99.4 104.2 92.9 3.8 1.5 7.6 6.5 3.4 7.6
Lasiocarpine 106.3 103.1 93.0 4.4 4.3 6.8 5.0 4.6 10.6
Scopolamine 83.9 102.5 90.7 8.9 3.5 7.8 9.4 8.1 7.8
Atropine 88.6 102.2 89.0 6.4 3.6 10.4 7.3 5.1 10.3
eISSN:
2450-8608
Langue:
Anglais
Périodicité:
4 fois par an
Sujets de la revue:
Life Sciences, Molecular Biology, Microbiology and Virology, other, Medicine, Veterinary Medicine
RSS Feed de la revue