Development of a Method Based on DLLME and UFLC-DAD for the Determination of Antibiotics in Honey Samples and the Study of Their Degradation Kinetics

Abstract

In this work, a method was developed, based on dispersive liquid-liquid microextraction (DLLME) and analysis by ultra-fast liquid chromatography coupled to diode array detector (UFLC-DAD), to simultaneously determine ten antibiotics of two different classes in honey, as well as to evaluate their degradation kinetics in this matrix. The extraction was optimized by a Box-Behnken design and the method provided good linearity and precision, limits of detection (LODs) in the range of 3.1-6.8 µg kg-1 and recoveries between 82.9 and 105.7%. The decay velocities along the storage period have followed a first order model for nine antibiotics, while one has fitted a zero order model. In the analysis of 33 samples, sulfadimethoxine and tetracycline were found in four samples of the same year and type of blooming, freshly produced in different places, at concentrations, respectively, below and 79% higher than the established by the Brazilian legislation. This suggests an application of those drugs to the beehives, probably shortly before the samples were taken.

Antibiotic residues in honey: a public health issue

“…According to the results presented, the proposed method was adequate in terms of linearity, precision, and LQ (Santana et al, 2018). However, it is important to note that the antibiotic levels found in the honey samples evaluated are worrying, given the high concentration of these substances found (Santana et al, 2018).…”

“…The authors report the presence of sulfadimethoxine in three samples at concentrations between 21.2 and 38.5 µg kg -1 , whereas tetracycline was found in only one sample (35.8 µg kg -1 ) (Santana et al, 2018). According to the results presented, the proposed method was adequate in terms of linearity, precision, and LQ (Santana et al, 2018). However, it is important to note that the antibiotic levels found in the honey samples evaluated are worrying, given the high concentration of these substances found (Santana et al, 2018).…”

“…In this sense, a method using DLLME as a way to prepare honey samples followed by the determination of 10 antibiotics by HPLC was developed by Santana et al (2018). In this work, 33 honey samples were evaluated for the presence of sulfathiazole, sulfadiazine, sulfamerazine, sulfamethazine, sulfamethoxazole, sulfadimethoxine, oxytetracycline, tetracycline, chlortetracycline, doxycycline, and their metabolites (Santana et al, 2018). The authors report the presence of sulfadimethoxine in three samples at concentrations between 21.2 and 38.5 µg kg -1 , whereas tetracycline was found in only one sample (35.8 µg kg -1 ) (Santana et al, 2018).…”

“…In this work, 33 honey samples were evaluated for the presence of sulfathiazole, sulfadiazine, sulfamerazine, sulfamethazine, sulfamethoxazole, sulfadimethoxine, oxytetracycline, tetracycline, chlortetracycline, doxycycline, and their metabolites (Santana et al, 2018). The authors report the presence of sulfadimethoxine in three samples at concentrations between 21.2 and 38.5 µg kg -1 , whereas tetracycline was found in only one sample (35.8 µg kg -1 ) (Santana et al, 2018). According to the results presented, the proposed method was adequate in terms of linearity, precision, and LQ (Santana et al, 2018).…”

“…2020; Bonerba et al, 2021; Galyautdinova et al, 2020;Kivrak et al, 2016;Korkmaz et al, 2017; 2020; Louppis, Kontominas, & Papastephanou, 2017; Mahmoudi, Norian, & Pajohi-Alamoti, 2014; Santana, Santana, & Pereira, 2018; Thanasarakhan et al, 2011) Sulphonamides (Baeza Fonte, Castro, & Liva-Garrido, 2018; Chiesa, Panseri, Nobile, Ceriani, & Arioli, 2018;Galarini et al, 2015;Kivrak et al, 2016;Korkmaz et al, 2017;Kümmerer, 2009;Louppis et al, 2017;Mujić et al, 2011;Santana et al, 2018; von Eyken et al., 2019) Aminoglycosides(Aksoy, 2019; Barrasso et al, 2018; Bonerba et al, 2021;Ji et al, 2013;Li, Li, Wang, & Ji, 2018;Mahmoudi et al, 2014;Perkons, Pugajeva, & Bartkevics, 2018;Wang et al, 2015) Macrolides(Aksoy, 2019; Alla, 2020; Bonerba et al, 2021;Du et al, 2018;Mahmoudi et al, 2014; …”