Abstract:A high-performance liquid chromatography-tandem quadrupole electrostatic-ion-trap high-resolution mass spectrometry (Q Exactive HF, HRMS) method with mixed-mode-adsorbent-based purification was established for the simultaneous determination of sulfaquinoxaline and diaveridine in eggs. The egg samples were first extracted by ultrasonic solvent extraction, followed by centrifugation of the extracts at 8000 r/min, and purification and collection via the addition of adsorbents with different operating mechanisms. The extracts were subsequently dried under nitrogen at 40 ℃, followed by the addition of 0.1% formic acid-acetonitrile solution (9:1, V/V) to prepare constant-volume samples suitable for mass spectrometry. An Acquity ultra-performance liquid chromatography (UPLC) Beh C18 (2.1 mm×100 mm, 1.7 μm) column was employed for separation, with 0.1% formic acid-water and 0.1% formic acid-methanol being used as the mobile phases for gradient elution. Mass spectrometry was conducted in the parallel reaction monitoring mode for the quantitative analysis of the target compounds. The two investigated compounds could be adequately separated under the established chromatographic conditions. Acceptable linear relationships in the linear range, and correlation coefficients greater than 0.999 were obtained. Standard addition validation at addition levels of 10, 50, and 200 ng/g resulted in average recoveries of 96.4%~106.8% of the two compounds being obtained, with relative standard deviations (RSDs) of less than 7.1%. The limit of detection (LOD, S/N=3) and limit of quantification (LOQ, S/N=10) of the developed method were found to be 0.1~0.2 μg/kg and 0.3~0.6 μg/kg, respectively. This method requires straightforward sample processing and enables a short duration of analysis, while ensuring accuracy, reliability, and high sensitivity, thereby establishing its suitability for the simultaneous determination of sulfaquinoxaline and sulfonamide potentiators in eggs.
