Use of a new LC-MS method for the determination of pyrrolizidine alkaloids in feeds
and | Jul 07, 2018
About this article
Published Online: Jul 07, 2018
Page range: 183 - 191
Received: Feb 08, 2018
Accepted: Jun 08, 2018
DOI: https://doi.org/10.2478/jvetres-2018-0028
Keywords
© 2018 Ewelina Kowalczyk et al., published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.
Fig. 1
Fig. 2
Fig. 3
Selected (m/z) ions and retention times of the monitored alkaloids. Determination coefficients obtained for matrix calibration curves in a concentration range corresponding to 0 – 100 μg kg-1 for all analysed alkaloids, and results of matrix effect evaluation. PA – pyrrolizidine alkaloid, RT – retention time, R2– coefficient of determination, ME – matrix effect
| PA | m/z | RT | R2 | ME (%) |
|---|---|---|---|---|
| Intermedine | 300.1 | 6.14 | 0.999 | 99.9 |
| Lycopsamine | 300.0 | 6.37 | 0.999 | 108.6 |
| Jacobine | 352.1 | 6.88 | 0.999 | 93.7 |
| Retrorsine | 352.1 | 8.29 | 0.996 | 98.3 |
| Heliotrine | 314.1 | 8.58 | 0.999 | 102.2 |
| Seneciphylline | 334.1 | 9.11 | 0.998 | 98.9 |
| Senecionine | 336.1 | 11.09 | 0.998 | 100.3 |
| Echimidine | 398.0 | 13.11 | 0.997 | 100.6 |
| Senkirkine | 366.1 | 13.37 | 0.997 | 89.9 |
| Lasiocarpine | 412.1 | 15.03 | 0.995 | 101.4 |
Validation parameters evaluated for ten alkaloids in feed matrix
| Concentration level (μg kg-1) | Concentration level (μg kg-1) | Concentration level (μg kg-1) | |||||||
|---|---|---|---|---|---|---|---|---|---|
| 5 | 20 | 100 | 5 | 20 | 100 | 5 | 20 | 100 | |
| PA | Recovery (%) | Repeatability RSD (%) | Reproducibility RSD (%) | ||||||
| Intermedine | 99.5 | 99.1 | 89.9 | 11.7 | 13.4 | 11.2 | 18.4 | 16.8 | 13.9 |
| Lycopsamine | 89.1 | 97.9 | 87.6 | 9.6 | 11.6 | 12.8 | 18.3 | 10.6 | 16.8 |
| Jacobine | 99.8 | 102.5 | 92.3 | 9.3 | 13.6 | 9.5 | 10.8 | 13.7 | 9.8 |
| Retrorsine | 112.9 | 84.1 | 97.1 | 10.1 | 10.9 | 4.0 | 16.3 | 18.9 | 4.8 |
| Heliotrine | 100.5 | 93.9 | 92.9 | 5.7 | 11.8 | 5.2 | 16.3 | 14.1 | 5.3 |
| Seneciphylline | 102.3 | 100.2 | 97.1 | 9.5 | 12.2 | 4.3 | 18.8 | 12.7 | 5.2 |
| Senecionine | 100.6 | 104.6 | 94.7 | 8.7 | 12.9 | 4.5 | 14.6 | 13.4 | 5.5 |
| Echimidine | 110.8 | 109.5 | 95.0 | 7.4 | 8.9 | 7.0 | 13.9 | 11.8 | 5.5 |
| Senkirkine | 94.2 | 106.4 | 97.5 | 3.0 | 5.6 | 5.9 | 18.0 | 9.9 | 8.0 |
| Lasiocarpine | 100.5 | 99.4 | 97.2 | 6.0 | 7.9 | 3.8 | 11.6 | 15.1 | 6.3 |