Determination of polypeptide antibiotics in animal tissues using liquid chromatography tandem mass spectrometry based on in-line molecularly imprinted solid-phase extraction

Autor: Xuqin, Song, Esther, Turiel, Jian, Yang, Antonio, Martín-Esteban, Limin, He
Přispěvatelé: National Science Foundation of China, National Natural Science Foundation of Guizhou University, Turiel, Esther, Martín-Esteban, Antonio
Jazyk: angličtina
Rok vydání: 2022
Předmět:
Popis: Effective purification and enrichment of polypeptide antibiotics in animal tissues is always a challenge, due to the co-extraction of other endogenous peptides which usually interfere their final determination. In this study, a molecularly imprinted column was prepared by packing polymyxin E-imprinted particles into a 100 mm × 4.6 mm i.d. HPLC column. The as-prepared imprinted columns were able to tolerate 100% aqueous phase and exhibited good stability and high column efficiency. Polypeptides antibiotics with similar molecular size or spatial structure to polymyxin E were well retained by the imprinted column, suggesting class selectivity. After optimization of mobile phase conditions of imprinted column, polypeptide antibiotics in animal tissue extracts were enriched and cleaned up by in-line molecularly imprinted solid-phase extraction, allowing the screening of target analytes in complex samples at low concentration levels by UV detection. Eluate fraction from the imprinted column was collected, and further dried and re-dissolved with methanol-0.5% formic acid aqueous solution (80:20, v/v) for final LC-MS/MS analysis. Analysis was accomplished using multiple reaction monitoring (MRM) in positive electrospray ionization mode and analytes quantified using the matrix-matched external calibration curves. The results showed high correlation coefficients for target analytes in the linear range of 2 ∼ 200 μg kg-1. At four different concentration levels (limit of quantification, 50, 100 and 200 μg kg-1), recoveries of four polypeptide antibiotics in swine, cattle and chicken muscles ranged from 66.7 to 94.5% with relative standard deviations lower than 16.0%. The limits of detection (LOD) were 2.0 ∼ 4.0 μg/kg, depending upon the analyte and sample. Compared with a conventional pretreatment method, the imprinted column was able to remove more impurities and to significantly reduce matrix effects, allowing the accurate analysis of polypeptide antibiotics.
This research was funded by the National Science Foundation of China (grant number 31572562), the Key Pro gram of Guangzhou Science and Technology Plan (grant number 201804020019) and the Special Funds of the National Natural Sci ence Foundation of Guizhou University ([2020]25)
Databáze: OpenAIRE