Development of a semi-automated one-step purification method for determination of 63 pesticides in fish samples by HPLC-MS/MS using natural loofah sponge as a novel adsorbent.

In this study, we developed a miniaturized semi-automatic purification method based on pressure-filtration purification for sensitive HPLC-MS/MS monitoring of pesticides in aquatic products. For the first time, loofah sponge was demonstrated and utilized as a novel green, low-cost, and effective one-step purification adsorbent for fish sample. The developed method consisted of two main steps: first, target analytes were extracted from fish samples using an acetonitrile-based QuEChERS extraction method. Subsequently, the extract was automatically purified through a pressure-filtration purification column in a centrifuge, followed by HPLC-MS/MS analysis. Under optimized experimental conditions, the method exhibited excellent linearity, with a range of 0.5 to 50.0 μg/L and a correlation coefficient > 0.99. The detection and quantification limits were 0.1-1.0 and 1.0-2.0 μg/kg, respectively. Recoveries at spiked levels of 2.0, 5.0 and 30.0 μg/kg ranged from 69.95 to 107.92%, with intra-day RSDs ranging from 0.58 to 15.01 % and inter-day RSDs ranging from 0.72 % to 14.32 %.