Dispersive liquid-liquid microextraction/HPLC techniques for determination of oxytetracycline and doxycycline residues in beef samples: method developments and statistical analysis
A rapid, cost-effective and environment-friendly sample pre-treatment method involving dispersive liquid-liquid microextraction (DLLME) and high-performance liquid chromatography (HPLC) was developed and applied for the extraction of oxytetracycline and doxycycline residues in beef samples (liver, k...
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| Format: | Article |
| Language: | English |
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Nigerian Society of Physical Sciences
2023-04-01
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| Series: | African Scientific Reports |
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| Online Access: | https://asr.nsps.org.ng/index.php/asr/article/view/87 |
| _version_ | 1827359033915342848 |
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| author | Muinat Aliu Abibat Junaid Abdulrahman Ibraheem Aisha Ishaq Abubakar Lawal Kikelomo Ayeni` Amudalat Lawal Lukman Abdulra'uf |
| author_facet | Muinat Aliu Abibat Junaid Abdulrahman Ibraheem Aisha Ishaq Abubakar Lawal Kikelomo Ayeni` Amudalat Lawal Lukman Abdulra'uf |
| author_sort | Muinat Aliu |
| collection | DOAJ |
| description | A rapid, cost-effective and environment-friendly sample pre-treatment method involving dispersive liquid-liquid microextraction (DLLME) and high-performance liquid chromatography (HPLC) was developed and applied for the extraction of oxytetracycline and doxycycline residues in beef samples (liver, kidney and muscle). Several influencing factors associated with the extraction and separation of these antibiotics residues, such as sample size, type and volume of disperser and extraction solvents, centrifugation speed and time, were optimized using Plackett-Burman design and central composite design, while insignificant factors were fixed at values determined using univariate analysis. Figures of merit of the analytical methodology including the limit of detection (LOD), the limit of quantification (LOQ), accuracy (in terms of average recoveries), precision and calibration functions were established according to the European Union commission decision 2002/657/EC. Linearity, in the range of 5–500 µg/kg, was obtained with regression coefficients ranging from 0.9983 – 0.9999. Inter-day repeatability, intra-day precision, LODs and LOQs obtained were 3.81 – 14.90%, 3.80 – 8.70%, 4.21 – 4.69 µg/kg and 14.02 – 15.65 µg/kg respectively. Samples with detectable drug residues have oxytetracycline being the most commonly detected. The developed method was successfully established and the concentration levels of drug residues detected were lower than the European Union set maximum residue level (MRL). |
| first_indexed | 2024-03-08T06:19:51Z |
| format | Article |
| id | doaj.art-dbaf5b6d289e4c4dad7aa88d84abf998 |
| institution | Directory Open Access Journal |
| issn | 2955-1625 2955-1617 |
| language | English |
| last_indexed | 2024-03-08T06:19:51Z |
| publishDate | 2023-04-01 |
| publisher | Nigerian Society of Physical Sciences |
| record_format | Article |
| series | African Scientific Reports |
| spelling | doaj.art-dbaf5b6d289e4c4dad7aa88d84abf9982024-02-04T08:39:15ZengNigerian Society of Physical SciencesAfrican Scientific Reports2955-16252955-16172023-04-01878710.46481/asr.2023.2.1.8787Dispersive liquid-liquid microextraction/HPLC techniques for determination of oxytetracycline and doxycycline residues in beef samples: method developments and statistical analysisMuinat Aliu0Abibat Junaid1Abdulrahman Ibraheem2Aisha Ishaq3Abubakar Lawal4Kikelomo Ayeni`5Amudalat Lawal6Lukman Abdulra'uf7Department of Chemistry and Industrial Chemistry, Faculty of Pure and Applied Sciences, Kwara State University, Malete, P.M.B 1530, Ilorin, Nigeria.Department of Chemistry and Industrial Chemistry, Faculty of Pure and Applied Sciences, Kwara State University, Malete, P.M.B 1530, Ilorin, Nigeria.Department of Chemistry and Industrial Chemistry, Faculty of Pure and Applied Sciences, Kwara State University, Malete, P.M.B 1530, Ilorin, NigeriaDepartment of Chemistry and Industrial Chemistry, Faculty of Pure and Applied Sciences, Kwara State University, Malete, P.M.B 1530, Ilorin, NigeriaDepartment of Pure and Industrial Chemistry, Umaru Musa Yar’adua University Katsina, NigeriaDepartment of Chemistry and Industrial Chemistry, Faculty of Pure and Applied Sciences, Kwara State University, Malete, P.M.B 1530, Ilorin, NigeriaDepartment of Biology, School of Sciences, Kwara State College of Education, Ilorin, NigeriaDepartment of Chemistry and Industrial Chemistry, Faculty of Pure and Applied Sciences, Kwara State University, Malete, P.M.B 1530, Ilorin, Nigeria.A rapid, cost-effective and environment-friendly sample pre-treatment method involving dispersive liquid-liquid microextraction (DLLME) and high-performance liquid chromatography (HPLC) was developed and applied for the extraction of oxytetracycline and doxycycline residues in beef samples (liver, kidney and muscle). Several influencing factors associated with the extraction and separation of these antibiotics residues, such as sample size, type and volume of disperser and extraction solvents, centrifugation speed and time, were optimized using Plackett-Burman design and central composite design, while insignificant factors were fixed at values determined using univariate analysis. Figures of merit of the analytical methodology including the limit of detection (LOD), the limit of quantification (LOQ), accuracy (in terms of average recoveries), precision and calibration functions were established according to the European Union commission decision 2002/657/EC. Linearity, in the range of 5–500 µg/kg, was obtained with regression coefficients ranging from 0.9983 – 0.9999. Inter-day repeatability, intra-day precision, LODs and LOQs obtained were 3.81 – 14.90%, 3.80 – 8.70%, 4.21 – 4.69 µg/kg and 14.02 – 15.65 µg/kg respectively. Samples with detectable drug residues have oxytetracycline being the most commonly detected. The developed method was successfully established and the concentration levels of drug residues detected were lower than the European Union set maximum residue level (MRL).https://asr.nsps.org.ng/index.php/asr/article/view/87beefliquid chromatographymicroextractiontetracyclinesvalidation` |
| spellingShingle | Muinat Aliu Abibat Junaid Abdulrahman Ibraheem Aisha Ishaq Abubakar Lawal Kikelomo Ayeni` Amudalat Lawal Lukman Abdulra'uf Dispersive liquid-liquid microextraction/HPLC techniques for determination of oxytetracycline and doxycycline residues in beef samples: method developments and statistical analysis African Scientific Reports beef liquid chromatography microextraction tetracyclines validation` |
| title | Dispersive liquid-liquid microextraction/HPLC techniques for determination of oxytetracycline and doxycycline residues in beef samples: method developments and statistical analysis |
| title_full | Dispersive liquid-liquid microextraction/HPLC techniques for determination of oxytetracycline and doxycycline residues in beef samples: method developments and statistical analysis |
| title_fullStr | Dispersive liquid-liquid microextraction/HPLC techniques for determination of oxytetracycline and doxycycline residues in beef samples: method developments and statistical analysis |
| title_full_unstemmed | Dispersive liquid-liquid microextraction/HPLC techniques for determination of oxytetracycline and doxycycline residues in beef samples: method developments and statistical analysis |
| title_short | Dispersive liquid-liquid microextraction/HPLC techniques for determination of oxytetracycline and doxycycline residues in beef samples: method developments and statistical analysis |
| title_sort | dispersive liquid liquid microextraction hplc techniques for determination of oxytetracycline and doxycycline residues in beef samples method developments and statistical analysis |
| topic | beef liquid chromatography microextraction tetracyclines validation` |
| url | https://asr.nsps.org.ng/index.php/asr/article/view/87 |
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