A QuEChERS method based on amino-functionalized halloysite nanotubes coupled with gas chromatography-tandem mass spectrometry for the quantification of 16 pesticides in three typical high-risk vegetables

In this study, a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the simultaneous quantification of 16 pesticide residues in three typical vegetable matrices, using amino-functionalized halloysite nanotubes (HNTs-NQ-62) as a novel cleanup adsorbent. Three modified HNTs, namely HNTs-KH-540, HNTs-KH-792, and HNTs-NQ-62, were synthesized and systematically compared. The results demonstrated that HNTs-NQ-62 yielded lower matrix effects (MEs) values than HNTs-KH-540 and HNTs-KH-792 and exhibited a greater capacity to alleviate matrix interferences. Method validation confirmed that the proposed method achieved favorable linearity, with correlation coefficients ( R 2 ) higher than 0.9989 for all target pesticides. The limits of detection (LODs) and quantification (LOQs) ranged from 0.02 to 1.5 μg/kg and from 0.06 to 5.0 μg/kg, respectively. Satisfactory recoveries of 80.8%-113.7% were obtained, while the intraday and interday relative standard deviations (RSDs) were below 8.8% and 7.2%, respectively. Comparative tests further revealed that HNTs-NQ-62 performed better than the commercial adsorbent in mitigating MEs to a certain extent. This study indicates that HNTs-NQ-62 holds a great promise as a favorable alternative to conventional QuEChERS cleanup adsorbents and that the developed method provides reliable analytical performance for the quantification of the 16 target pesticides in vegetable matrices.