Determination of Tetracycline, Oxytetracycline, Sulfadiazine, Norfloxacin, and Enrofloxacin in Swine Manure Using a Coupled Method of On-Line Solid-Phase Extraction with the UHPLC-DAD

Mohamed S Gaballah; Xin Li; Zijia Zhang; Abdulaziz Al-Anazi; Hui Sun; Mostafa Sobhi; Mperejekumana Philbert; Mohamed A Ghorab; Jianbin Guo; Renjie Dong

doi:10.3390/antibiotics10111397

Determination of Tetracycline, Oxytetracycline, Sulfadiazine, Norfloxacin, and Enrofloxacin in Swine Manure Using a Coupled Method of On-Line Solid-Phase Extraction with the UHPLC-DAD

Antibiotics (Basel). 2021 Nov 13;10(11):1397. doi: 10.3390/antibiotics10111397.

Authors

Mohamed S Gaballah^{1

2}, Xin Li¹, Zijia Zhang¹, Abdulaziz Al-Anazi³, Hui Sun¹, Mostafa Sobhi⁴, Mperejekumana Philbert¹, Mohamed A Ghorab^{5

6}, Jianbin Guo¹, Renjie Dong^{1

7}

Affiliations

¹ Bioenergy and Environment Science & Technology Laboratory, College of Engineering, China Agricultural University, Beijing 100083, China.
² Department of Marine Environment, National Institute of Oceanography and Fisheries, NIOF, Alexandria 21556, Egypt.
³ Department of Chemical Engineering, College of Engineering, King Saud University (KSU), P.O. Box 800, Riyadh 11421, Saudi Arabia.
⁴ Agricultural and Bio-Systems Engineering Department, Faculty of Agriculture, Alexandria University, Alexandria 21511, Egypt.
⁵ Office of Chemical Safety and Pollution Prevention, U.S. Environmental Protection Agency (EPA), Washington, DC 20004, USA.
⁶ Wildlife Toxicology Laboratory, Department of Animal Science, Institute for Integrative Toxicology (IIT), Michigan State University, East Lansing, MI 48824, USA.
⁷ Yantai Institute, China Agricultural University, Yantai 264032, China.

Abstract

The use of various veterinary antibiotics (VAs) in animal husbandry raises serious concerns about the development of antibiotic resistance. Antibiotics such as tetracycline, oxytetracycline, sulfadiazine, norfloxacin, and enrofloxacin are the most frequently used antimicrobial compounds in animal husbandry and generate large eco-toxicological effects; however, they are still difficult to determine in a complex matrix such as swine manure. This study has developed an effective method for detecting five VAs in swine manure using Ultra-High-Performance Liquid Chromatography-Diode Array Detector (UHPLC-DAD) coupled with on-line solid-phase extraction (SPE). The results show that the mobile phase of ACN/0.01 M oxalic acid was the optimum at pH 3.0. VAs in a swine manure matrix were extracted using solid extraction buffer solution (T3) with 97.36% recovery. Sensitivity, accuracy, and precision were also evaluated. The validity study showed good linearity (R² > 0.99). Limit of detection (LOD) was found to be from 0.1 to 0.42 µg mL^-1 in the liquid fraction and from 0.032 to 0.58 µg g^-1 dw in the solid fraction. The corresponding values of the limit of quantification (LOQ) ranged from 0.32 to 1.27 µg mL^-1 for the liquid fraction and from 0.096 to 1.77 µg g^-1 dw for the solid fraction. Therefore, the proposed method showed the potential applicability for detecting different antibiotic compounds from swine manure samples.

Keywords: UHPLC; on-line SPE; swine manure; veterinary antibiotics.