Development and Validation of a Method for the Analysis of Multiple Pesticides in Fishery Products Using Gas Chromatography with Micro-Electron Capture Detection and Gas Chromatography–Tandem Mass Spectrometry
This study aims to develop a simultaneous analytical method for detecting 19 pesticides, including 4,4′-DDD, in fishery products using gas chromatography with micro-electron capture detection (GC-μECD) and gas chromatography–tandem mass spectrometry (GC-MS/MS). A new analytical method was developed...
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2025-05-01
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| author | Myungheon Kim Mihyun Cho Changkyo Seo Jaebin Im Changhyeon Park Yoonmi Lee Mi-Ra Jo Yong-Sun Moon Moo-Hyeog Im |
| author_facet | Myungheon Kim Mihyun Cho Changkyo Seo Jaebin Im Changhyeon Park Yoonmi Lee Mi-Ra Jo Yong-Sun Moon Moo-Hyeog Im |
| author_sort | Myungheon Kim |
| collection | DOAJ |
| description | This study aims to develop a simultaneous analytical method for detecting 19 pesticides, including 4,4′-DDD, in fishery products using gas chromatography with micro-electron capture detection (GC-μECD) and gas chromatography–tandem mass spectrometry (GC-MS/MS). A new analytical method was developed to measure pesticide residues in fishery products based on the modified Association of Official Analytical Chemists protocol combining quick, easy, cheap, effective, rugged, and safe (QuEChERS) and the Pesticide Analytical Manual for extraction and purification. Extraction was performed using acetonitrile containing 0.1% acetic acid, and purification was conducted with Florisil cartridges. The Florisil cartridges were more effective than QuEChERS in removing impurities and pigments during purification and also resulted in a reduced matrix effect. The validation followed Codex guidelines (CAC/GL 40). The limit of detection ranged from 2 to 3 ng/g, and the limit of quantification (LOQ) from 7 to 10 ng/g. Matrix-matched calibration curves exhibited linearity with coefficients of determination exceeding 0.99 for all target analytes. Accuracy was assessed based on recovery rates, while precision was evaluated using relative standard deviations (RSD) at three spiking levels (LOQ, 10×LOQ, and 50×LOQ). The recovery rates ranged from 62.6 to 119.1%, with RSDs of 0.4 to 19.5%, conforming to Codex guidelines. |
| format | Article |
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| institution | Kabale University |
| issn | 2297-8739 |
| language | English |
| publishDate | 2025-05-01 |
| publisher | MDPI AG |
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| spelling | doaj-art-c0068ed7809f40599aade167908efcfb2025-08-20T03:27:26ZengMDPI AGSeparations2297-87392025-05-0112614210.3390/separations12060142Development and Validation of a Method for the Analysis of Multiple Pesticides in Fishery Products Using Gas Chromatography with Micro-Electron Capture Detection and Gas Chromatography–Tandem Mass SpectrometryMyungheon Kim0Mihyun Cho1Changkyo Seo2Jaebin Im3Changhyeon Park4Yoonmi Lee5Mi-Ra Jo6Yong-Sun Moon7Moo-Hyeog Im8Department of Food Engineering, Daegu University, Gyeongsan 38453, Republic of KoreaDepartment of Food Engineering, Daegu University, Gyeongsan 38453, Republic of KoreaDepartment of Food Engineering, Daegu University, Gyeongsan 38453, Republic of KoreaDepartment of Food Engineering, Daegu University, Gyeongsan 38453, Republic of KoreaDepartment of Food Engineering, Daegu University, Gyeongsan 38453, Republic of KoreaFood Safety and Processing Research Division, National Institute Fisheries Science, Busan 46083, Republic of KoreaFood Safety and Processing Research Division, National Institute Fisheries Science, Busan 46083, Republic of KoreaDepartment of Horticulture and Life Science, Yeungnam University, Gyeongsan 38541, Republic of KoreaDepartment of Food Engineering, Daegu University, Gyeongsan 38453, Republic of KoreaThis study aims to develop a simultaneous analytical method for detecting 19 pesticides, including 4,4′-DDD, in fishery products using gas chromatography with micro-electron capture detection (GC-μECD) and gas chromatography–tandem mass spectrometry (GC-MS/MS). A new analytical method was developed to measure pesticide residues in fishery products based on the modified Association of Official Analytical Chemists protocol combining quick, easy, cheap, effective, rugged, and safe (QuEChERS) and the Pesticide Analytical Manual for extraction and purification. Extraction was performed using acetonitrile containing 0.1% acetic acid, and purification was conducted with Florisil cartridges. The Florisil cartridges were more effective than QuEChERS in removing impurities and pigments during purification and also resulted in a reduced matrix effect. The validation followed Codex guidelines (CAC/GL 40). The limit of detection ranged from 2 to 3 ng/g, and the limit of quantification (LOQ) from 7 to 10 ng/g. Matrix-matched calibration curves exhibited linearity with coefficients of determination exceeding 0.99 for all target analytes. Accuracy was assessed based on recovery rates, while precision was evaluated using relative standard deviations (RSD) at three spiking levels (LOQ, 10×LOQ, and 50×LOQ). The recovery rates ranged from 62.6 to 119.1%, with RSDs of 0.4 to 19.5%, conforming to Codex guidelines.https://www.mdpi.com/2297-8739/12/6/142method developmentfishery productsGC-μECDGC-MS/MSpesticide |
| spellingShingle | Myungheon Kim Mihyun Cho Changkyo Seo Jaebin Im Changhyeon Park Yoonmi Lee Mi-Ra Jo Yong-Sun Moon Moo-Hyeog Im Development and Validation of a Method for the Analysis of Multiple Pesticides in Fishery Products Using Gas Chromatography with Micro-Electron Capture Detection and Gas Chromatography–Tandem Mass Spectrometry Separations method development fishery products GC-μECD GC-MS/MS pesticide |
| title | Development and Validation of a Method for the Analysis of Multiple Pesticides in Fishery Products Using Gas Chromatography with Micro-Electron Capture Detection and Gas Chromatography–Tandem Mass Spectrometry |
| title_full | Development and Validation of a Method for the Analysis of Multiple Pesticides in Fishery Products Using Gas Chromatography with Micro-Electron Capture Detection and Gas Chromatography–Tandem Mass Spectrometry |
| title_fullStr | Development and Validation of a Method for the Analysis of Multiple Pesticides in Fishery Products Using Gas Chromatography with Micro-Electron Capture Detection and Gas Chromatography–Tandem Mass Spectrometry |
| title_full_unstemmed | Development and Validation of a Method for the Analysis of Multiple Pesticides in Fishery Products Using Gas Chromatography with Micro-Electron Capture Detection and Gas Chromatography–Tandem Mass Spectrometry |
| title_short | Development and Validation of a Method for the Analysis of Multiple Pesticides in Fishery Products Using Gas Chromatography with Micro-Electron Capture Detection and Gas Chromatography–Tandem Mass Spectrometry |
| title_sort | development and validation of a method for the analysis of multiple pesticides in fishery products using gas chromatography with micro electron capture detection and gas chromatography tandem mass spectrometry |
| topic | method development fishery products GC-μECD GC-MS/MS pesticide |
| url | https://www.mdpi.com/2297-8739/12/6/142 |
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