Development and validation of a solid‐phase extraction method coupled with LC–MS/MS for the simultaneous determination of 16 antibiotic residues in duck meat

Abstract

The present study was carried out to determine 16 antibiotics belonging to seven different groups (tetracyclines, sulfonamides, penicillins, fluoroquinolones, macrolides, lincosamides and trimethoprims) in duck meat. A solid‐phase extraction method based on Oasis HLB cartridges coupled with liquid chromatography–electrospray ionization tandem mass spectrometry was developed. Solutions of 0.1 m ethylenediaminetetraacetic acid disodium salt and 2% trifluoroacetic acid were used for the preliminary extraction of the target antibiotics from duck meat and n‐hexane was used for purification prior to solid‐phase extraction. Mobile phases composed of 0.1% trifluoroacetic acid in distilled water (solvent A) and 0.1% trifluoroacetic acid in methanol (solvent B), combined with a reversed‐phase C18 analytical column, provided the optimal separation and signal intensity. The linearity of the method was assessed using six concentrations (5, 10, 20, 30, 40, and 50 μg/kg), and the recoveries, which were calculated at three spiking concentrations (5, 10 and 20 μg/kg), were in the range 69.8–103.3% with relative standard deviations (RSDs) ≤ 6.9% for the 16 tested antibiotics. Matrix effects ranging from −47.2 to −13.5% were observed for all the analytes, and the limits of quantitation (LOQ), which ranged from 4.93 to 26.21 μg/kg, were much lower than the maximum residue limits (MRLs) set by various regulatory authorities. Ten samples from a market were tested, and none of the target analytes were detected. Thus, a simple and versatile protocol has been developed to detect and quantify 16 antibiotics in duck meat samples.

Determination of antibiotics in meat samples using analytical methodologies: A review

“…For multi‐class analysis, ACN has been used to extract some antibiotics from different meat tissues (Saito‐Shida, Sakai, Nemoto, & Akiyama, 2017; Tajabadi, Ghambarian, Yamini, & Yazdanfar, 2016) sometimes combined with water (Casey, Andersen, Williams, Nickel, & Ayres, 2020; Lehotay & Lightfield, 2018; Moretti et al., 2016; Song et al., 2017; Yin et al., 2016; Y. Zhang et al., 2018), EDTA (Dasenaki, Michali, & Thomaidis, 2016; Moretti et al., 2016; Yin et al., 2016; Zhao, Lucas, Long, Richter, & Stevens, 2018; Zheng et al., 2019), aqueous ammonium solutions (Dasenaki et al., 2016; Kang et al., 2017), TCA (Dasenaki et al., 2016; Rizzetti, de Souza, Prestes, Adaime, & Zanella, 2017), formic acid (He, Song, Zhou, & Zhao, 2017; Pugajeva, Ikkere, Judjallo, & Bartkevics, 2019; L. Zhao et al., 2018), dimethyl sulfoxide (Zhao et al., 2018), acetic acid (M. Zhang et al., 2018), or ethyl acetate (Yoshikawa et al., 2017). In addition, other solvents such as MeOH with formic acid (Danezis, Anagnostopoulos, Liapis, & Koupparis, 2016) or EDTA (Arslanbaş, 2018), PBS (Oyedeji, Msagati, Williams, & Benson, 2020) with TCA (Sarker et al., 2018), or McIlvaine buffer (Zhang et al., 2016) have been used.…”

“…Some of these methods are used in routine laboratories to control the presence of residues in animal origin tissues. For multi-class analysis, ACN has been used to extract some antibiotics from different meat tissues (Saito-Shida, Sakai, Nemoto, & Akiyama, 2017;Tajabadi, Ghambarian, Yamini, & Yazdanfar, 2016) sometimes combined with water (Casey, Andersen, Williams, Nickel, & Ayres, 2020;Lehotay & Lightfield, 2018;Moretti et al, 2016;Song et al, 2017;Yin et al, 2016;, EDTA (Dasenaki, Michali, & Thomaidis, 2016;Moretti et al, 2016;Yin et al, 2016;Zhao, Lucas, Long, Richter, & Stevens, 2018;Zheng et al, 2019), aqueous ammonium solutions (Dasenaki et al, 2016;Kang et al, 2017), TCA (Dasenaki et al, 2016;Rizzetti, de Souza, Prestes, Adaime, & Zanella, 2017), formic acid (He, Song, Zhou, & Zhao, 2017;Pugajeva, Ikkere, Judjallo, & Bartkevics, 2019;L. Zhao et al, 2018), dimethyl sulfoxide (Zhao et al, 2018), acetic acid (M. , or ethyl acetate (Yoshikawa et al, 2017).…”

“…In addition, other solvents such as MeOH with formic acid (Danezis, Anagnostopoulos, Liapis, & Koupparis, 2016) or EDTA (Arslanbaş, 2018), PBS (Oyedeji, Msagati, Williams, & Benson, 2020) with TCA (Sarker et al, 2018), or McIlvaine buffer (Zhang et al, 2016) have been used. For enrichment and purification steps, the use of traditional SPE (Dasenaki et al, 2016;Oyedeji et al, 2020;Pugajeva et al, 2019;Saito-Shida et al, 2017;Yoshikawa et al, 2017;Zhang et al, 2016;Zhao et al, 2018;Zheng et al, 2019), DSPE (Casey et al, 2020;Kang et al, 2017), MSPD , MISPE (Song et al, 2017), QuEChERS (Chen, Pan, Huang, Han, & Zhou, 2019;Desmarchelier et al, 2018;Jammoul & Darra, 2019;Qin et al, 2017), and hollow fiber-based liquid phase microextraction (Tajabadi et al, 2016) have been described. For multi-residue determination, LC coupled to MS is the most used technique (Casey et al, 2020;Danezis et al, 2016;Dasenaki et al, 2016;Desmarchelier et al, 2018;Jammoul & Darra, 2019;Kang et al, 2017;Lehotay & Lightfield, 2018;Moretti et al, 2016;Pugajeva et al, 2019;Qin et al, 2017;Rizzeti et al, 2017;Saito-Shida et al, 2017;Yin et al, 2016;Yoshikawa et al, 2017;…”

Simple, fast and reliable CE method for simultaneous determination of ciprofloxacin and ofloxacin in human urine

“…These are, for example, animal food additives or medicines given to animals. It is commonly known that antibiotics are increasingly being used in animal husbandry due to the need for rapid growth of animals 1 , 2 . Excretion of the residues of these compounds with animal urine and feces leads to environmental pollution 1 , 3 , 4 .…”

“…This is a very unfavorable phenomenon because infections caused by antibiotic-resistant bacteria are very difficult to cure, sometimes even impossible 5 . Therefore, maximum residue limits have been established for veterinary antibiotics in food of animal origin 1 , 2 , 6 .…”