Matrix-induced sugaring-out liquid–liquid extraction for the determination of fumagillin and dicyclohexylamine residues in honey by LC–MS/MS
Abstract The dicyclohexylamine salt of fumagillin is currently used in some countries to control nosema disease in honey bee colonies. Chemical residues in honey resulting from the use of chemotherapies in apiculture are a food safety concern. A method employing matrix-induced sugaring-out liquid–li...
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Springer
2025-07-01
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| Series: | Discover Food |
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| Online Access: | https://doi.org/10.1007/s44187-025-00522-3 |
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| author | Thomas S. Thompson Johan P. van den Heever Melissa J. Zarft |
| author_facet | Thomas S. Thompson Johan P. van den Heever Melissa J. Zarft |
| author_sort | Thomas S. Thompson |
| collection | DOAJ |
| description | Abstract The dicyclohexylamine salt of fumagillin is currently used in some countries to control nosema disease in honey bee colonies. Chemical residues in honey resulting from the use of chemotherapies in apiculture are a food safety concern. A method employing matrix-induced sugaring-out liquid–liquid extraction (SULLE) with LC–MS/MS detection was developed for the determination of fumagillin and dicyclohexylamine (DCH) residues. Honey was dissolved in water and extracted with acetonitrile where the high concentration of sugars in the sample matrix enabled phase separation of the two solvents and partitioning of the analytes into the organic layer. The working analytical range spanned 5 to 500 µg kg−1 with limits of detection (LOD) estimated to be 1.7 and 1.4 µg kg−1 for fumagillin and DCH, respectively. Method validation experiments using blank replicate honey samples fortified with 5, 25, 150, and 400 µg kg−1 of each analyte were carried out over multiple days. Average accuracies ranged from 86.6 to 106.3% and 95.2 to 108.8% for fumagillin and DCH, respectively. Intra- and inter-day precisions were less than 20% at the limit of quantitation (LOQ) concentration of 5 µg kg−1 and less than 10% at all other studied concentrations. The analytical method was applied to the determination of fumagillin and DCH residues in 464 honey samples. Fumagillin was found in 28 samples at concentrations from 5 to 74 µg kg−1. Residues of DCH were observed more frequently (265 samples) at concentrations ranging from 5 to 219 µg kg−1. |
| format | Article |
| id | doaj-art-ca19360a00a74c3ebae7e18e65cd1b4f |
| institution | Kabale University |
| issn | 2731-4286 |
| language | English |
| publishDate | 2025-07-01 |
| publisher | Springer |
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| series | Discover Food |
| spelling | doaj-art-ca19360a00a74c3ebae7e18e65cd1b4f2025-08-20T03:43:02ZengSpringerDiscover Food2731-42862025-07-015111610.1007/s44187-025-00522-3Matrix-induced sugaring-out liquid–liquid extraction for the determination of fumagillin and dicyclohexylamine residues in honey by LC–MS/MSThomas S. Thompson0Johan P. van den Heever1Melissa J. Zarft2Agri-Food Assurance Section, Food Safety Branch, Alberta Agriculture and IrrigationAgri-Food Assurance Section, Food Safety Branch, Alberta Agriculture and IrrigationAgri-Food Assurance Section, Food Safety Branch, Alberta Agriculture and IrrigationAbstract The dicyclohexylamine salt of fumagillin is currently used in some countries to control nosema disease in honey bee colonies. Chemical residues in honey resulting from the use of chemotherapies in apiculture are a food safety concern. A method employing matrix-induced sugaring-out liquid–liquid extraction (SULLE) with LC–MS/MS detection was developed for the determination of fumagillin and dicyclohexylamine (DCH) residues. Honey was dissolved in water and extracted with acetonitrile where the high concentration of sugars in the sample matrix enabled phase separation of the two solvents and partitioning of the analytes into the organic layer. The working analytical range spanned 5 to 500 µg kg−1 with limits of detection (LOD) estimated to be 1.7 and 1.4 µg kg−1 for fumagillin and DCH, respectively. Method validation experiments using blank replicate honey samples fortified with 5, 25, 150, and 400 µg kg−1 of each analyte were carried out over multiple days. Average accuracies ranged from 86.6 to 106.3% and 95.2 to 108.8% for fumagillin and DCH, respectively. Intra- and inter-day precisions were less than 20% at the limit of quantitation (LOQ) concentration of 5 µg kg−1 and less than 10% at all other studied concentrations. The analytical method was applied to the determination of fumagillin and DCH residues in 464 honey samples. Fumagillin was found in 28 samples at concentrations from 5 to 74 µg kg−1. Residues of DCH were observed more frequently (265 samples) at concentrations ranging from 5 to 219 µg kg−1.https://doi.org/10.1007/s44187-025-00522-3FumagillinDicyclohexylamineHoneySugaring-out liquid–liquid extractionLC–MS/MS |
| spellingShingle | Thomas S. Thompson Johan P. van den Heever Melissa J. Zarft Matrix-induced sugaring-out liquid–liquid extraction for the determination of fumagillin and dicyclohexylamine residues in honey by LC–MS/MS Discover Food Fumagillin Dicyclohexylamine Honey Sugaring-out liquid–liquid extraction LC–MS/MS |
| title | Matrix-induced sugaring-out liquid–liquid extraction for the determination of fumagillin and dicyclohexylamine residues in honey by LC–MS/MS |
| title_full | Matrix-induced sugaring-out liquid–liquid extraction for the determination of fumagillin and dicyclohexylamine residues in honey by LC–MS/MS |
| title_fullStr | Matrix-induced sugaring-out liquid–liquid extraction for the determination of fumagillin and dicyclohexylamine residues in honey by LC–MS/MS |
| title_full_unstemmed | Matrix-induced sugaring-out liquid–liquid extraction for the determination of fumagillin and dicyclohexylamine residues in honey by LC–MS/MS |
| title_short | Matrix-induced sugaring-out liquid–liquid extraction for the determination of fumagillin and dicyclohexylamine residues in honey by LC–MS/MS |
| title_sort | matrix induced sugaring out liquid liquid extraction for the determination of fumagillin and dicyclohexylamine residues in honey by lc ms ms |
| topic | Fumagillin Dicyclohexylamine Honey Sugaring-out liquid–liquid extraction LC–MS/MS |
| url | https://doi.org/10.1007/s44187-025-00522-3 |
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