Optimization and Validation of a QuEChERS-Based Method Combined with Gas Chromatography–Tandem Mass Spectrometry for Analyzing Pesticide Residues in Edible Insect Samples
The increasing popularity of edible insects as a sustainable food source necessitates stringent safety measures to monitor pesticide contamination. This study aimed to assess and enhance a QuEChERS-based extraction method coupled with gas chromatography–tandem mass spectrometry (GC-MS/MS) for the qu...
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2025-05-01
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| author | Phannika Tongchai Nootchakarn Sawarng Anurak Wongta Udomsap Jaitham Kunrunya Sutan Saweang Kawichai Chuleui Jung Bajaree Chuttong Surat Hongsibsong |
| author_facet | Phannika Tongchai Nootchakarn Sawarng Anurak Wongta Udomsap Jaitham Kunrunya Sutan Saweang Kawichai Chuleui Jung Bajaree Chuttong Surat Hongsibsong |
| author_sort | Phannika Tongchai |
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| description | The increasing popularity of edible insects as a sustainable food source necessitates stringent safety measures to monitor pesticide contamination. This study aimed to assess and enhance a QuEChERS-based extraction method coupled with gas chromatography–tandem mass spectrometry (GC-MS/MS) for the quantification of pesticide residues in edible insects (bamboo caterpillars, house crickets, silkworm pupae, giant water bugs, and grasshoppers) by combining multiple individual insect specimens into a single, homogenized sample—five replicates were tested. The method was optimized by evaluating various extraction parameters and showed strong linearity for all 47 target pesticides, with correlation coefficients (R<sup>2</sup>) ranging from 0.9940 to 0.9999. The limits of detection (LODs) varied between 1 and 10 µg/kg, while the limits of quantification (LOQs) ranged from 10 to 15 µg/kg. Recovery studies conducted at three fortification levels (10, 100, and 500 µg/kg) revealed recoveries ranging from 64.54% to 122.12%, that over 97.87% of the pesticides exhibited satisfactory recoveries within the range of 70–120%, and relative standard deviations (RSDs) below 20%, between 1.86% and 6.02%. Matrix effects (%MEs) range from −33.01% to 24.04%, and to those that experienced no effect. More than 94% of the analytes showed minimal ion suppression or enhancement. These results conform to the SANTE guidelines for monitoring pesticide residues in edible insects, enhancing food safety standards and safeguarding consumer protection. |
| format | Article |
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| institution | Kabale University |
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| language | English |
| publishDate | 2025-05-01 |
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| series | Molecules |
| spelling | doaj-art-b23f7aca4a8e46a09431d24a622603f52025-08-20T03:46:53ZengMDPI AGMolecules1420-30492025-05-013011229310.3390/molecules30112293Optimization and Validation of a QuEChERS-Based Method Combined with Gas Chromatography–Tandem Mass Spectrometry for Analyzing Pesticide Residues in Edible Insect SamplesPhannika Tongchai0Nootchakarn Sawarng1Anurak Wongta2Udomsap Jaitham3Kunrunya Sutan4Saweang Kawichai5Chuleui Jung6Bajaree Chuttong7Surat Hongsibsong8School of Health Sciences Research, Research Institute for Health Sciences, Chiang Mai University, Chiang Mai 50200, ThailandFaculty of Public Health, Chiang Rai Rajabhat University, Chiang Rai 57100, ThailandSchool of Health Sciences Research, Research Institute for Health Sciences, Chiang Mai University, Chiang Mai 50200, ThailandSchool of Health Sciences Research, Research Institute for Health Sciences, Chiang Mai University, Chiang Mai 50200, ThailandEnvironmental, Occupational Health Sciences and NCD Center of Excellence, Research Institute for Health Sciences, Chiang Mai University, Chiang Mai 50200, ThailandEnvironmental, Occupational Health Sciences and NCD Center of Excellence, Research Institute for Health Sciences, Chiang Mai University, Chiang Mai 50200, ThailandDepartment of Plant Medicals, Gyeongkuk National University, Andong 36729, Republic of KoreaMeliponini and Apini Research Laboratory, Department of Entomology and Plant Pathology, Faculty of Agriculture, Chiang Mai University, Chiang Mai 50200, ThailandSchool of Health Sciences Research, Research Institute for Health Sciences, Chiang Mai University, Chiang Mai 50200, ThailandThe increasing popularity of edible insects as a sustainable food source necessitates stringent safety measures to monitor pesticide contamination. This study aimed to assess and enhance a QuEChERS-based extraction method coupled with gas chromatography–tandem mass spectrometry (GC-MS/MS) for the quantification of pesticide residues in edible insects (bamboo caterpillars, house crickets, silkworm pupae, giant water bugs, and grasshoppers) by combining multiple individual insect specimens into a single, homogenized sample—five replicates were tested. The method was optimized by evaluating various extraction parameters and showed strong linearity for all 47 target pesticides, with correlation coefficients (R<sup>2</sup>) ranging from 0.9940 to 0.9999. The limits of detection (LODs) varied between 1 and 10 µg/kg, while the limits of quantification (LOQs) ranged from 10 to 15 µg/kg. Recovery studies conducted at three fortification levels (10, 100, and 500 µg/kg) revealed recoveries ranging from 64.54% to 122.12%, that over 97.87% of the pesticides exhibited satisfactory recoveries within the range of 70–120%, and relative standard deviations (RSDs) below 20%, between 1.86% and 6.02%. Matrix effects (%MEs) range from −33.01% to 24.04%, and to those that experienced no effect. More than 94% of the analytes showed minimal ion suppression or enhancement. These results conform to the SANTE guidelines for monitoring pesticide residues in edible insects, enhancing food safety standards and safeguarding consumer protection.https://www.mdpi.com/1420-3049/30/11/2293pesticide residuesedible insectsQuEChERSGC-MS/MSfood safetymethod validation |
| spellingShingle | Phannika Tongchai Nootchakarn Sawarng Anurak Wongta Udomsap Jaitham Kunrunya Sutan Saweang Kawichai Chuleui Jung Bajaree Chuttong Surat Hongsibsong Optimization and Validation of a QuEChERS-Based Method Combined with Gas Chromatography–Tandem Mass Spectrometry for Analyzing Pesticide Residues in Edible Insect Samples Molecules pesticide residues edible insects QuEChERS GC-MS/MS food safety method validation |
| title | Optimization and Validation of a QuEChERS-Based Method Combined with Gas Chromatography–Tandem Mass Spectrometry for Analyzing Pesticide Residues in Edible Insect Samples |
| title_full | Optimization and Validation of a QuEChERS-Based Method Combined with Gas Chromatography–Tandem Mass Spectrometry for Analyzing Pesticide Residues in Edible Insect Samples |
| title_fullStr | Optimization and Validation of a QuEChERS-Based Method Combined with Gas Chromatography–Tandem Mass Spectrometry for Analyzing Pesticide Residues in Edible Insect Samples |
| title_full_unstemmed | Optimization and Validation of a QuEChERS-Based Method Combined with Gas Chromatography–Tandem Mass Spectrometry for Analyzing Pesticide Residues in Edible Insect Samples |
| title_short | Optimization and Validation of a QuEChERS-Based Method Combined with Gas Chromatography–Tandem Mass Spectrometry for Analyzing Pesticide Residues in Edible Insect Samples |
| title_sort | optimization and validation of a quechers based method combined with gas chromatography tandem mass spectrometry for analyzing pesticide residues in edible insect samples |
| topic | pesticide residues edible insects QuEChERS GC-MS/MS food safety method validation |
| url | https://www.mdpi.com/1420-3049/30/11/2293 |
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