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

doi:10.3390/antibiotics10111397

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.

Highlights

Veterinary antibiotics (VAs), including tetracyclines (TCs), sulfonamides (Sulfs), and fluoroquinolones (FQs), are frequently used to promote animal growth and prevent disease in the livestock industry [1,2]
This study aims to establish a simple but effective analytical method for determining five veterinary antibiotics (VAs) (TC, OTC, SDZ, Norf, and Enorf) from swine manure matrix, depending on an on-line solid-phase extraction (SPE) technique coupled with Ultra-High-Performance-Liquid Chromatography (UHPLC)–Diode array detectors (DAD)
270 and 277 nm were found to be suitable by delivering high peak values for the targeted VAs (Table 1)

Summary

Introduction

Veterinary antibiotics (VAs), including tetracyclines (TCs), sulfonamides (Sulfs), and fluoroquinolones (FQs), are frequently used to promote animal growth and prevent disease in the livestock industry [1,2]. Because of their widespread misuse and difficulty to digest in the animal’s gut, a certain amount of VAs is excreted into the animal’s feces [2,3]. China is one of the biggest VAs producers worldwide, with tetracycline accounting for half of all VAs produced each year (including antibiotics used in animal feed) [5]. Several recent studies used HPLC for TCs, sulfonamides, and FQs quantification in other animals’ matrices [9,10,11,12,13]

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Results

Conclusion