Dispersive Solid-Phase Extraction and Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry—A Rapid and Accurate Method for Detecting 10 Macrolide Residues in Aquatic Products
The amount of macrolide (MAL) residues in aquatic products, including oleandomycin (OLD), erythromycin (ERM), clarithromycin (CLA), azithromycin (AZI), kitasamycin (KIT), josamycin (JOS), spiramycin (SPI), tilmicosin (TIL), tylosin (TYL), and roxithromycin (ROX), was determined using solid-phase ext...
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| Format: | Article |
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MDPI AG
2024-03-01
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| Series: | Foods |
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| Online Access: | https://www.mdpi.com/2304-8158/13/6/866 |
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| author | Jinyu Chen Guangming Mei Xiaojun Zhang Daoxiang Huang Pengfei He Dan Xu |
| author_facet | Jinyu Chen Guangming Mei Xiaojun Zhang Daoxiang Huang Pengfei He Dan Xu |
| author_sort | Jinyu Chen |
| collection | DOAJ |
| description | The amount of macrolide (MAL) residues in aquatic products, including oleandomycin (OLD), erythromycin (ERM), clarithromycin (CLA), azithromycin (AZI), kitasamycin (KIT), josamycin (JOS), spiramycin (SPI), tilmicosin (TIL), tylosin (TYL), and roxithromycin (ROX), was determined using solid-phase extraction and ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS). The residues were extracted with 1% ammonia acetonitrile solution and purified by neutral alumina adsorption. Chromatographic separation was completed on an ACQUITY UPLC BEH C<sub>18</sub> column with acetonitrile–0.1% formic acid aqueous solution as the mobile phase, and mass spectrometry detection was performed by multiple reaction monitoring scanning with the positive mode in an electrospray ion source (ESI<sup>+</sup>). Five isotopically labeled compounds were used as internal standards for quality control purposes. The findings indicated that across the mass concentration span of 1.0–100 μg/L, there was a strong linear correlation (<i>R</i><sup>2</sup> > 0.99) between the concentration and instrumental response for the 10 MALs. The limit of detection of UPLC-MS/MS was 0.25–0.50 μg/kg, and the limit of quantitation was 0.5–1.0 μg/kg. The added recovery of blank matrix samples at standard gradient levels (1.0, 5.0, and 50.0 μg/kg) was 83.1–116.6%, and the intra-day precision and inter-day precisions were 3.7 and 13.8%, respectively. The method is simple and fast, with high accuracy and good repeatability, in line with the requirements for accurate qualitative and quantitative analysis of the residues for 10 MALs in aquatic products. |
| first_indexed | 2024-04-24T18:16:30Z |
| format | Article |
| id | doaj.art-09353cc960104500b31d7f0e518c9a02 |
| institution | Directory Open Access Journal |
| issn | 2304-8158 |
| language | English |
| last_indexed | 2024-04-24T18:16:30Z |
| publishDate | 2024-03-01 |
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| record_format | Article |
| series | Foods |
| spelling | doaj.art-09353cc960104500b31d7f0e518c9a022024-03-27T13:41:01ZengMDPI AGFoods2304-81582024-03-0113686610.3390/foods13060866Dispersive Solid-Phase Extraction and Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry—A Rapid and Accurate Method for Detecting 10 Macrolide Residues in Aquatic ProductsJinyu Chen0Guangming Mei1Xiaojun Zhang2Daoxiang Huang3Pengfei He4Dan Xu5College of Food and Pharmaceutical Science, Zhejiang Ocean University, Zhoushan 316022, ChinaZhejiang Marine Fisheries Research Institute, Zhoushan 316021, ChinaZhejiang Marine Fisheries Research Institute, Zhoushan 316021, ChinaCollege of Food and Pharmaceutical Science, Zhejiang Ocean University, Zhoushan 316022, ChinaZhejiang Marine Fisheries Research Institute, Zhoushan 316021, ChinaZhejiang Marine Fisheries Research Institute, Zhoushan 316021, ChinaThe amount of macrolide (MAL) residues in aquatic products, including oleandomycin (OLD), erythromycin (ERM), clarithromycin (CLA), azithromycin (AZI), kitasamycin (KIT), josamycin (JOS), spiramycin (SPI), tilmicosin (TIL), tylosin (TYL), and roxithromycin (ROX), was determined using solid-phase extraction and ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS). The residues were extracted with 1% ammonia acetonitrile solution and purified by neutral alumina adsorption. Chromatographic separation was completed on an ACQUITY UPLC BEH C<sub>18</sub> column with acetonitrile–0.1% formic acid aqueous solution as the mobile phase, and mass spectrometry detection was performed by multiple reaction monitoring scanning with the positive mode in an electrospray ion source (ESI<sup>+</sup>). Five isotopically labeled compounds were used as internal standards for quality control purposes. The findings indicated that across the mass concentration span of 1.0–100 μg/L, there was a strong linear correlation (<i>R</i><sup>2</sup> > 0.99) between the concentration and instrumental response for the 10 MALs. The limit of detection of UPLC-MS/MS was 0.25–0.50 μg/kg, and the limit of quantitation was 0.5–1.0 μg/kg. The added recovery of blank matrix samples at standard gradient levels (1.0, 5.0, and 50.0 μg/kg) was 83.1–116.6%, and the intra-day precision and inter-day precisions were 3.7 and 13.8%, respectively. The method is simple and fast, with high accuracy and good repeatability, in line with the requirements for accurate qualitative and quantitative analysis of the residues for 10 MALs in aquatic products.https://www.mdpi.com/2304-8158/13/6/866antibiotic residuemacrolidesolid-phase extractionisotopically labelled internal standardLC-MS/MS |
| spellingShingle | Jinyu Chen Guangming Mei Xiaojun Zhang Daoxiang Huang Pengfei He Dan Xu Dispersive Solid-Phase Extraction and Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry—A Rapid and Accurate Method for Detecting 10 Macrolide Residues in Aquatic Products Foods antibiotic residue macrolide solid-phase extraction isotopically labelled internal standard LC-MS/MS |
| title | Dispersive Solid-Phase Extraction and Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry—A Rapid and Accurate Method for Detecting 10 Macrolide Residues in Aquatic Products |
| title_full | Dispersive Solid-Phase Extraction and Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry—A Rapid and Accurate Method for Detecting 10 Macrolide Residues in Aquatic Products |
| title_fullStr | Dispersive Solid-Phase Extraction and Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry—A Rapid and Accurate Method for Detecting 10 Macrolide Residues in Aquatic Products |
| title_full_unstemmed | Dispersive Solid-Phase Extraction and Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry—A Rapid and Accurate Method for Detecting 10 Macrolide Residues in Aquatic Products |
| title_short | Dispersive Solid-Phase Extraction and Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry—A Rapid and Accurate Method for Detecting 10 Macrolide Residues in Aquatic Products |
| title_sort | dispersive solid phase extraction and ultra performance liquid chromatography tandem mass spectrometry a rapid and accurate method for detecting 10 macrolide residues in aquatic products |
| topic | antibiotic residue macrolide solid-phase extraction isotopically labelled internal standard LC-MS/MS |
| url | https://www.mdpi.com/2304-8158/13/6/866 |
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