Simultaneous Determination of Amphenicols and Metabolites in Animal-Derived Foods Using Ultrahigh-Performance Liquid Chromatography-Tandem Mass Spectrometry

Abstract

Amphenicols are widely used to prevent and treat animal diseases. However, amphenicol residues accumulate in livestock and poultry and harm consumers. We hypothesized that one can combine solid-phase extraction (SPE) with ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) to simultaneously determine amphenicols and metabolites in pork, beef, lamb, chicken, and their products and meet government regulations for maximum residue limits. We extracted crude samples with ethyl acetate and ammonia water (98:2, v/v), purified the samples with a CNW Si SPE column, defatted the samples with acetonitrile-saturated n-hexane, and then determined the resulting analytes by UHPLC-MS/MS. The limit of detection of the analytes in livestock and poultry meat was 0.03–1.50 μg/kg, and the limit of quantification was 0.05–5.00 μg/kg. Measured chloramphenicol, thiamphenicol, and florfenicol concentrations were linear over the range 0.50–50 μg/kg; and the florfenicol amine concentration was linear over the range 5.00–200 μg/kg (all with correlation coefficients >0.9990). The recovery of the spiked samples was between 72% and 120%. The intraday relative standard deviation (RSD) ranged from 1% to 9%, and the interday RSD ranged from 1% to 12%. Based on the above results, the current method is sensitive, accurate, and reproducible with the detection limits being well below the maximum residue limits as per Chinese standard GB 31650-2019, and thus, our research hypothesis could be confirmed.

Florfenicol and Florfenicol Amine Quantification in Bull Serum and Seminal Plasma by a Single Validated UHPLC‐MS/MS Method

“…A consistent part of the methods described in the literature employ organic solvents such as ethyl acetate [ 24 , 25 ], acetone, dichloromethane [ 26 ], and acetonitrile with or without formic acid [ 27 ], or alkaline pH conditions for FF extraction from different animal tissues or feed. Other published applications for its quantification in plasma and serum are based on multiple liquid-liquid and/or solid-phase extraction techniques [ 16 , 17 ].…”

Antibiogram profiles of pathogenic and commensal bacteria in goat and sheep feces on smallholder farm

“…Amphenicols, a group of broad-spectrum antibiotics primarily utilized in veterinary medicine, are employed for treating illnesses in agricultural animals (Trif et al, 2023). Notably, amphenicols, including chloramphenicol and florfenicol, are extensively utilized in livestock farming, leading to their accumulation in animals and posing risks to consumers (Wu et al, 2021). Moreover, chloramphenicol exhibits high toxicity towards the human hematopoietic system, potentially inducing adverse effects such as aplastic anemia (Cerutti et al, 2021).…”

Effect of Cooking Methods on Amphenicols and Metabolites Residues in Livestock and Poultry Meat Spiked Tissues

“…The extraction and purification of amphenicols and metabolites from livestock and poultry meat were performed using our self-built method [ 13 ]. Briefly, pork, beef, lamb and chicken samples were chopped and homogenized at 10,000 r/min using an HM6300 intelligent homogenizer (Lab Precision Beijing Technology Co., Ltd., Beijing, China).…”