Low-background interference detection of glyphosate, glufosinate, and AMPA in foods using UPLC-MS/MS without derivatization.

The abuse of herbicides has emerged as a great threat to food security. Herein, a low-background interference detection method based on UPLC-MS was developed for the simultaneous determination of glufosinate, glyphosate, and its metabolite aminomethylphosphonic acid (AMPA) in foods. Initially, this study proposed a simple and rapid pretreatment method, utilizing water extraction and PRiME HLB purification to isolate glyphosate, glufosinate, and AMPA from food samples. After the optimization of pretreatment conditions, the processed samples are then analyzed directly by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS) without pre-column derivatization. The method can effectively reduce interference from by-products of pre-column derivatization and background substrates of food sample, showing low matrix effects (ME) ranging from - 24.83 to 32.10%. Subsequently, the method has been validated by 13 kinds of food samples. The recoveries of the three herbicides in the food samples range from 84.2 to 115.6%. The limit of detection (LOD) is lower to 0.073 mg/kg, 0.017 mg/kg, and 0.037 mg/kg, respectively. Moreover, the method shows an excellent reproducibility with relative standard deviations (RSD) within 16.9%. Thus, the method can provide high trueness, reproducibility, sensitivity, and interference-free detection to ensure human health safety.

Preparation of a hydrophobic deep eutectic solvent and its application in the detection of quinolone residues in cattle urine.

Enrichment for the detection of quinolone residues is usually cumbersome and requires large amounts of toxic organic reagents. Therefore, this study synthesized a low-toxicity hydrophobic deep eutectic solvent (DES) with DL-menthol and p-cresol, which was then characterized by Fourier transform infrared spectroscopy, nuclear magnetic resonance, and thermal analysis. A simple and rapid vortex-assisted liquid-liquid microextraction method was developed based on this DES for the extraction of eight quinolones from cattle urine. The optimal extraction conditions were screened by examining the DES volume, extraction temperature, vortex time, and salt concentration. Under the optimal conditions, the linear ranges of the eight quinolones were 1 ~ 100 µg/L with good linearity (r2 was 0.998 ~ 0.999), and the limits of detection and quantification were 0.08 ~ 0.30 µg/L and 0.27 ~ 0.98 µg/L, respectively. The average extraction recoveries of spiked cattle urine samples were 70.13 ~ 98.50% with relative standard deviations below 13.97%. This method can provide a reference for the pre-treatment of quinolone residue detection.