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

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

Journal of Veterinary Research

Volume 66 (2022): Issue 2 (June 2022)

By: Ewelina Kowalczyk and Krzysztof Kwiatek

Open Access

|Jul 2022

Figures & Tables

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

Boxplots of the concentration of determined alkaloids

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

DOI: https://doi.org/10.2478/jvetres-2022-0032 | Journal eISSN: 2450-8608

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Language: English

Page range: 235 - 243

Submitted on: Jan 13, 2022

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Accepted on: Jun 20, 2022

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Published on: Jul 5, 2022

Published by: National Veterinary Research Institute in Pulawy

In partnership with: Paradigm Publishing Services

Publication frequency: 4 issues per year

Keywords:

pyrrolizidine alkaloids,

tropane alkaloids,

liquid chromatography–mass spectrometry (LC-MS),

solid-phase extraction

Related subjects:

Molecular biology,

Microbiology and virology,

Life sciences, other,

Veterinary medicine

© 2022 Ewelina Kowalczyk, Krzysztof Kwiatek, 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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