Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils
A greener sample preparation method based on magnetic solid phase microextraction (MSPμE) was developed for the preconcentration of neonicotinoid pesticides (acetamiprid, imidacloprid, thiacloprid and thiamethoxam) in vegetable oil samples followed by separation and quantification using high perform...
Saved in:
| Main Authors: | , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
Elsevier
2025-02-01
|
| Series: | Advances in Sample Preparation |
| Subjects: | |
| Online Access: | http://www.sciencedirect.com/science/article/pii/S2772582025000063 |
| Tags: |
Add Tag
No Tags, Be the first to tag this record!
|
| _version_ | 1832540404339179520 |
|---|---|
| author | Musiiwa V. Sengane Masixole Sihlahla Philiswa N. Nomngongo Nomvano Mketo |
| author_facet | Musiiwa V. Sengane Masixole Sihlahla Philiswa N. Nomngongo Nomvano Mketo |
| author_sort | Musiiwa V. Sengane |
| collection | DOAJ |
| description | A greener sample preparation method based on magnetic solid phase microextraction (MSPμE) was developed for the preconcentration of neonicotinoid pesticides (acetamiprid, imidacloprid, thiacloprid and thiamethoxam) in vegetable oil samples followed by separation and quantification using high performance liquid chromatography with diode array detector (HPLC-DAD). Different characterisation techniques such as Fourier Transform Infrared Spectroscopy (FTIR), Powder X-ray diffraction analysis (PXRD), Thermogravimetric Analysis (TGA), Transmission electron microscopy (TEM), and scanning electron microscope and energy-dispersive X-ray spectroscopy (SEM-EDS) confirmed the synthesised magnetic nano adsorbents (Fe3O4, Fe3O4@Al2O3 and Fe3O4@Al2O3/AC). The most influential parameters affecting MSPμE of NEOs by Fe3O4@Al2O3/AC were examined using a multivariate optimisation approach and 8 min extraction time, 13 pH, 9 mg adsorbent mass, and 0.5 mL eluent volume were optimal parameters. The proposed Fe3O4@Al2O3/AC method showed high accuracy (80–119.21%) and precision (≤10 %) for all the investigated NEOs. Additionally, the obtained limit of detection (LOD) ranged from 0.5–1.76 ng µL-1, the limit of quantification (LOQ) ranged from 1.87–6.62 ng µL-1 and satisfactory high preconcentration factors (73.02- 407.0) were comparable with literature reported studies. The Analytical GREEness calculator AGREE, BAGI and NEMI analysis confirmed greenness of MSPμE. After that, the validated MSPμE method was applied to real vegetable oil samples (avocado, canola, olive and sunflower), and fortunately, all the investigated NEOs were below LODs of the proposed MSPμE /HPLC-DAD methods. |
| format | Article |
| id | doaj-art-874ddc610e814d77bb93773538754235 |
| institution | Kabale University |
| issn | 2772-5820 |
| language | English |
| publishDate | 2025-02-01 |
| publisher | Elsevier |
| record_format | Article |
| series | Advances in Sample Preparation |
| spelling | doaj-art-874ddc610e814d77bb937735387542352025-02-05T04:32:52ZengElsevierAdvances in Sample Preparation2772-58202025-02-0113100152Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oilsMusiiwa V. Sengane0Masixole Sihlahla1Philiswa N. Nomngongo2Nomvano Mketo3Department of Chemistry, College of Science and Engineering and Technology, Florida Science Campus, University of South Africa, Roodepoort, 1710, Johannesburg, South AfricaDepartment of Chemistry, College of Science and Engineering and Technology, Florida Science Campus, University of South Africa, Roodepoort, 1710, Johannesburg, South AfricaDepartment of Chemical Sciences, University of Johannesburg, PO Box 17011, Doornfontein 2028, Johannesburg, South AfricaDepartment of Chemistry, College of Science and Engineering and Technology, Florida Science Campus, University of South Africa, Roodepoort, 1710, Johannesburg, South Africa; Corresponding author.A greener sample preparation method based on magnetic solid phase microextraction (MSPμE) was developed for the preconcentration of neonicotinoid pesticides (acetamiprid, imidacloprid, thiacloprid and thiamethoxam) in vegetable oil samples followed by separation and quantification using high performance liquid chromatography with diode array detector (HPLC-DAD). Different characterisation techniques such as Fourier Transform Infrared Spectroscopy (FTIR), Powder X-ray diffraction analysis (PXRD), Thermogravimetric Analysis (TGA), Transmission electron microscopy (TEM), and scanning electron microscope and energy-dispersive X-ray spectroscopy (SEM-EDS) confirmed the synthesised magnetic nano adsorbents (Fe3O4, Fe3O4@Al2O3 and Fe3O4@Al2O3/AC). The most influential parameters affecting MSPμE of NEOs by Fe3O4@Al2O3/AC were examined using a multivariate optimisation approach and 8 min extraction time, 13 pH, 9 mg adsorbent mass, and 0.5 mL eluent volume were optimal parameters. The proposed Fe3O4@Al2O3/AC method showed high accuracy (80–119.21%) and precision (≤10 %) for all the investigated NEOs. Additionally, the obtained limit of detection (LOD) ranged from 0.5–1.76 ng µL-1, the limit of quantification (LOQ) ranged from 1.87–6.62 ng µL-1 and satisfactory high preconcentration factors (73.02- 407.0) were comparable with literature reported studies. The Analytical GREEness calculator AGREE, BAGI and NEMI analysis confirmed greenness of MSPμE. After that, the validated MSPμE method was applied to real vegetable oil samples (avocado, canola, olive and sunflower), and fortunately, all the investigated NEOs were below LODs of the proposed MSPμE /HPLC-DAD methods.http://www.sciencedirect.com/science/article/pii/S2772582025000063Neonicotinoid pesticidesVegetable oilsMagnetic solid phase microextraction (MSPμE)HPLC-DADAGREEFe3O4@Al2O3/AC |
| spellingShingle | Musiiwa V. Sengane Masixole Sihlahla Philiswa N. Nomngongo Nomvano Mketo Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils Advances in Sample Preparation Neonicotinoid pesticides Vegetable oils Magnetic solid phase microextraction (MSPμE) HPLC-DAD AGREE Fe3O4@Al2O3/AC |
| title | Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils |
| title_full | Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils |
| title_fullStr | Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils |
| title_full_unstemmed | Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils |
| title_short | Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils |
| title_sort | greener and rapid magnetic solid phase microextraction method using fe3o4 al2o3 ac for chromatographic determination of neonicotinoid pesticides in vegetable oils |
| topic | Neonicotinoid pesticides Vegetable oils Magnetic solid phase microextraction (MSPμE) HPLC-DAD AGREE Fe3O4@Al2O3/AC |
| url | http://www.sciencedirect.com/science/article/pii/S2772582025000063 |
| work_keys_str_mv | AT musiiwavsengane greenerandrapidmagneticsolidphasemicroextractionmethodusingfe3o4al2o3acforchromatographicdeterminationofneonicotinoidpesticidesinvegetableoils AT masixolesihlahla greenerandrapidmagneticsolidphasemicroextractionmethodusingfe3o4al2o3acforchromatographicdeterminationofneonicotinoidpesticidesinvegetableoils AT philiswannomngongo greenerandrapidmagneticsolidphasemicroextractionmethodusingfe3o4al2o3acforchromatographicdeterminationofneonicotinoidpesticidesinvegetableoils AT nomvanomketo greenerandrapidmagneticsolidphasemicroextractionmethodusingfe3o4al2o3acforchromatographicdeterminationofneonicotinoidpesticidesinvegetableoils |