Development and application of a simultaneous quantitative analysis method of 58 pesticide residues in Anemarrhena asphodeloides based on QuEChERS- GC-QQQ-MS/MS / 中草药

ABSTRACT

Objective: To establish a simultaneous quantitative analysis method of 58 pesticide residues in Anemarrhena asphodeloides based on QuEChERS-GC-QQQ-MS/MS technique. Methods: This study was performed on a Shimadzu GC-QQQ-MS/MS spectrometer, equipped with a SHIMADZU SH-Rxi-5Sil MS column (30 m × 0.25 mm, 0.25 μm). The temperature of injection port was 250 ℃, the injection volume was 1.0 μL, the injection mode was splitless, the injection pressure was 250 kPa; The carrier gas was high purity helium and the carrier gas control mode was constant linear velocity mode; The column flow rate was 1.69 mL/min, the line speed was 47.2 cm/s, the purge flow rate was 5 mL/min. The temperature rise method was the gradient program The initial temperature was 50 ℃, hold the state for 1 min, first raise the temperature to 125 ℃ with 25 ℃/min, then raise the temperature to 300 ℃ with 10 ℃/min, keep the state for 15 min; The balance time was 0.5 min. The QuEChERS method was used to purify the test sample solutions, and the calibration was carried out using the standard curve of blank matrix matching, using a stable isotope internal standard for quantitative. Results: Quantitative determination of 58 pesticide residues in 30 batches of A. asphodeloides samples was carried out. The results showed that there were five batches of samples detecting a small amount of p,p’-DDE, three batches of samples were detected trifluralin, two batches of samples were detected chlorpyrifos, and one batch of samples were detected butralin. Conclusion: The development and validation quantitative analysis method of 58 pesticide residues based on QuEChERS-GC-QQQ-MS/MS has good applicability, which is of reference value for the establishment of other pesticide residues in herbs.