Establishment of modified QuEChERS-GC-MS-LC-MS/MS method for simultaneous screening of multi-class multi-pesticide residues in betelvine and consumer risk assessment

Betelvine (Piper betel L.) in India is grown as an important cash crop with great demand in several countries. Due to its raw intake, the presence of undesirable pesticides in betelvine is an alarming issue of global concern. Therefore, a reliable method is needed to monitor their residues. In this study, a modified QuEChERS method was developed and validated to screen fifty-seven (57) widely used multi-class pesticide residues using gas chromatography-mass spectrometry (GC-MS) and liquid chromatography with tandem mass spectrometry (LC-MS/ MS). The sample was extracted with acetonitrile and cleaned in dispersive solid-phase extraction (dSPE) with graphitized carbon black (GCB) + primary secondary amine (PSA) + Florosil, PSA + C18, and C18 + GCB sorbent combinations to assess matrix interference cleanup efficiencies. The optimized method produced remarkable linearity from 0.01 to 1.0 mgL(-1) with satisfactory limits of quantification from 0.01 to 0.05 mgL-1. The best-spiked recovery of target analytes in the GCB + PSA + Florosil combination was 70-120% with precision RPDs < 17.97%, demonstrating good adsorption ability for co-extractives. Matrix effect (ME) values ranged between-19.74% and + 23.6%. Collected market samples (75) from the designated districts of West Bengal, India were screened and 9% were found to be contaminated with some non-recommended pesticides like carbendazim and tebuconazole. Human risk indexes (HRI) of the determined xenobiotics were also estimated (0.007 to 0.62), which were fortunately within the acceptable limit (HRI < 1.0). So, the developed modified QuEChERS method might be beneficial for quick and accurate screening of multi-class multi-pesticide residues in betelvine intended for export and food safety.

Automated summary

This study developed a modified QuEChERS method for the quick and accurate screening of multi-class multi-pesticide residues in betelvine. 9% of the collected market samples were found to be contaminated with non-recommended pesticides, but the human risk indexes were within the acceptable range.