Experimental Design Assisted HPLC/UV and LC-MS/MS for Simultaneous Determination of Selected Veterinary Antibiotics in Broiler Chicken

Antibiotics are used in the poultry industry to treat and prevent diseases. Their frequent use resulted in the appearance of antibiotic residuals in poultry meat, which is considered a serious public health issue. Among frequently used antibiotics are cefotaxime (CTX), ciprofloxacin (CIP), colistin...

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Main Authors: Mohamed A. Abdelshakour, Aziza E. Mostafa, Ghada M. Hadad, Dalia M. Hamed, Omayma M. El-Darder, Alaa El-Gindy, Roaa M. Khinkar, Mohammed M. Aldurdunji, Samar S. Murshid, Randa A. Abdel Salam
Format: Article
Language:English
Published: MDPI AG 2022-12-01
Series:Separations
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Online Access:https://www.mdpi.com/2297-8739/9/12/427
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author Mohamed A. Abdelshakour
Aziza E. Mostafa
Ghada M. Hadad
Dalia M. Hamed
Omayma M. El-Darder
Alaa El-Gindy
Roaa M. Khinkar
Mohammed M. Aldurdunji
Samar S. Murshid
Randa A. Abdel Salam
author_facet Mohamed A. Abdelshakour
Aziza E. Mostafa
Ghada M. Hadad
Dalia M. Hamed
Omayma M. El-Darder
Alaa El-Gindy
Roaa M. Khinkar
Mohammed M. Aldurdunji
Samar S. Murshid
Randa A. Abdel Salam
author_sort Mohamed A. Abdelshakour
collection DOAJ
description Antibiotics are used in the poultry industry to treat and prevent diseases. Their frequent use resulted in the appearance of antibiotic residuals in poultry meat, which is considered a serious public health issue. Among frequently used antibiotics are cefotaxime (CTX), ciprofloxacin (CIP), colistin (CST), doxycycline (DOX), flumequine (FLU), sulfamethoxazole (SMZ), trimethoprim (TMP) and tylosin (TYL). This study aimed to develop an optimized and validated method for concurrent estimation of the eight antibiotics in broiler chicken samples based on an easy extraction method followed by HPLC-UV and LC/MS/MS analysis. An experimental design was used for the optimization of the extraction procedure. Optimal conditions for separation were determined by using a central composite design after studying (1) mobile phase initial concentration, (2) column temperature, and (3) flow rate. The method was validated on the bases of ICH guidelines. The detection limits ranged from 3 to 5 µg kg<sup>−1</sup> for HPLC- UV and ranged from 0.01 to 0.05 µg kg<sup>−1</sup> for LC/MS/MS, while quantification limits ranged from 10 to 16 µg kg<sup>−1</sup> for HPLC- UV and ranged from 0.01 to 0.11 µg kg<sup>−1</sup> for LC/MS/MS. The chromatographic techniques were utilized for the analysis of spiked broiler chicken samples at a concentration range from 30 to 300 µg kg<sup>−1</sup>) for HPLC-UV and 0.01–20 µg kg<sup>−1</sup> for LC/MS/MS. The proposed methods were used for quantification of the residues of the studied antibiotics in real broiler samples obtained from local supermarkets in Ismailia governorate, Egypt. The detected levels of residual antibiotics were within the permissible limits.
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spelling doaj.art-292b150e174d468cb98ba0f00ea5ec002023-11-24T17:59:54ZengMDPI AGSeparations2297-87392022-12-0191242710.3390/separations9120427Experimental Design Assisted HPLC/UV and LC-MS/MS for Simultaneous Determination of Selected Veterinary Antibiotics in Broiler ChickenMohamed A. Abdelshakour0Aziza E. Mostafa1Ghada M. Hadad2Dalia M. Hamed3Omayma M. El-Darder4Alaa El-Gindy5Roaa M. Khinkar6Mohammed M. Aldurdunji7Samar S. Murshid8Randa A. Abdel Salam9Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Sohag University, Sohag 82524, EgyptDepartment of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Suez Canal University, Ismailia 41522, EgyptDepartment of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Suez Canal University, Ismailia 41522, EgyptDepartment of Avian and Rabbit Medicine, Faculty of Veterinary Medicine, Suez Canal University, Ismailia 41522, EgyptDepartment of Home Economics, Faculty of Education, Suez Canal University, Ismailia 41522, EgyptDepartment of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Suez Canal University, Ismailia 41522, EgyptDepartment of Pharmacy Practice, Faculty of Pharmacy, King Abdulaziz University, Jeddah 21589, Saudi ArabiaDepartment of Clinical Pharmacy, College of Pharmacy, Umm Al-Qura University, P.O. Box 13578, Makkah 21955, Saudi ArabiaDepartment of Natural Products, Faculty of Pharmacy, King Abdulaziz University, Jeddah 21589, Saudi ArabiaDepartment of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Suez Canal University, Ismailia 41522, EgyptAntibiotics are used in the poultry industry to treat and prevent diseases. Their frequent use resulted in the appearance of antibiotic residuals in poultry meat, which is considered a serious public health issue. Among frequently used antibiotics are cefotaxime (CTX), ciprofloxacin (CIP), colistin (CST), doxycycline (DOX), flumequine (FLU), sulfamethoxazole (SMZ), trimethoprim (TMP) and tylosin (TYL). This study aimed to develop an optimized and validated method for concurrent estimation of the eight antibiotics in broiler chicken samples based on an easy extraction method followed by HPLC-UV and LC/MS/MS analysis. An experimental design was used for the optimization of the extraction procedure. Optimal conditions for separation were determined by using a central composite design after studying (1) mobile phase initial concentration, (2) column temperature, and (3) flow rate. The method was validated on the bases of ICH guidelines. The detection limits ranged from 3 to 5 µg kg<sup>−1</sup> for HPLC- UV and ranged from 0.01 to 0.05 µg kg<sup>−1</sup> for LC/MS/MS, while quantification limits ranged from 10 to 16 µg kg<sup>−1</sup> for HPLC- UV and ranged from 0.01 to 0.11 µg kg<sup>−1</sup> for LC/MS/MS. The chromatographic techniques were utilized for the analysis of spiked broiler chicken samples at a concentration range from 30 to 300 µg kg<sup>−1</sup>) for HPLC-UV and 0.01–20 µg kg<sup>−1</sup> for LC/MS/MS. The proposed methods were used for quantification of the residues of the studied antibiotics in real broiler samples obtained from local supermarkets in Ismailia governorate, Egypt. The detected levels of residual antibiotics were within the permissible limits.https://www.mdpi.com/2297-8739/9/12/427antibioticsfood analysisliquid chromatographysustainability of natural resources
spellingShingle Mohamed A. Abdelshakour
Aziza E. Mostafa
Ghada M. Hadad
Dalia M. Hamed
Omayma M. El-Darder
Alaa El-Gindy
Roaa M. Khinkar
Mohammed M. Aldurdunji
Samar S. Murshid
Randa A. Abdel Salam
Experimental Design Assisted HPLC/UV and LC-MS/MS for Simultaneous Determination of Selected Veterinary Antibiotics in Broiler Chicken
Separations
antibiotics
food analysis
liquid chromatography
sustainability of natural resources
title Experimental Design Assisted HPLC/UV and LC-MS/MS for Simultaneous Determination of Selected Veterinary Antibiotics in Broiler Chicken
title_full Experimental Design Assisted HPLC/UV and LC-MS/MS for Simultaneous Determination of Selected Veterinary Antibiotics in Broiler Chicken
title_fullStr Experimental Design Assisted HPLC/UV and LC-MS/MS for Simultaneous Determination of Selected Veterinary Antibiotics in Broiler Chicken
title_full_unstemmed Experimental Design Assisted HPLC/UV and LC-MS/MS for Simultaneous Determination of Selected Veterinary Antibiotics in Broiler Chicken
title_short Experimental Design Assisted HPLC/UV and LC-MS/MS for Simultaneous Determination of Selected Veterinary Antibiotics in Broiler Chicken
title_sort experimental design assisted hplc uv and lc ms ms for simultaneous determination of selected veterinary antibiotics in broiler chicken
topic antibiotics
food analysis
liquid chromatography
sustainability of natural resources
url https://www.mdpi.com/2297-8739/9/12/427
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