Green and Efficient Determination of Fluoroquinolone Residues in Edible Green Fruits and Leafy Vegetables by Ultrasound-Assisted Extraction Followed by HPLC-MS/MS

Abstract

In this work, a simple, quick and efficient analytical method for determination of human and veterinary fluoroquinolone antimicrobial residues in lettuce, cucumber and spinach is developed. The procedure entails a 6 min ultrasound-assisted extraction (UAE, 3 × 2 min) in an alkaline (2% v/v NH3) aqueous solution containing Mg2+ ions (3 × 6 mL), with no need for organic solvents. The extract is submitted to cleanup on the HLB™ cartridge and the fluoroquinolones are separated and quantified by HPLC-MS/MS in a 10 min chromatographic run, using a small amount of acetonitrile in the mobile phase. The method, entirely developed in real matrices, is validated according to the updated analytical guidelines and provided suitable recoveries in the range of 67–116% and precision (RSD ≤ 20%, n = 3) at different concentrations (15, 70 and 150 ng g−1), with method quantification limits of 2–10 ng g−1. Fluoroquinolones were detected and quantified at concentrations from few to hundreds of nanograms per gram in vegetables from supermarkets, demonstrating the applicability of the method for monitoring residues of these pharmaceuticals.

Exploring the Potential of Microextraction in the Survey of Food Fruits and Vegetable Safety

“…Regarding antibiotics, three works were found employing UAE with commercially available SPE cartridges. Tadic et al [95] extracted ten antibiotics from different vegetables (lettuce, tomato, cauliflower, broad beans) using the Strata-X SPE cartridge, while Merlo et al [96] and Hu et al [9] employed the Oasis PRiME HLB cartridges to extract and quantified seven antibiotics from vegetables and 81 antibiotics from banana and cabbage samples, respectively. The most ideal LODs, in the range 0.001-0.26 ng g −1 , were achieved by Hu et al [9], which were certainly boosted by the higher sensitivity of the analytical instruments used (UHPLC-MS/MS).…”

Efficient Sequential Detection of Two Antibiotics Using a Fiber-Optic Surface Plasmon Resonance Sensor

“…Among these, fiber-optic SPR sensors have attracted significant attention due to their miniaturization and portability [31]. Although some conventional analytical techniques, including high-performance liquid chromatography (HPLC) [32], mass spectrometry (MS) [33], ELISA [34], SERS [35], etc., have been developed and applied to analyze substances' compositions, these techniques' various drawbacks limit their application in complex environments [36]. SPR sensors can provide higher analytical accuracy with a smaller sample amount [37].…”