Validation of LC-MS/MS method for simultaneous determination of chlorpyrifos, deltamethrin, imidacloprid and some of their metabolites in maize silage

Abstract

In this study, a validation of a multi-residue analysis method was performed for the simultaneous analysis of chlorpyrifos (CHL), deltamethrin (DEL) and Imidacloprid (IMI) residues and some of their metabolites in maize silage, by LC MS/MS. Extraction was conducted with acetonitrile acidified with 1% acetic acid. To avoid the matrix effect, a matrix matched calibration was used. The method was validated according to the SANTE/12682/2019 Guidelines. Selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), trueness (recovery %) and precision (intra-day and inter-day) parameters were evaluated in line with the SANTE document. The linearities of all compounds were quite confident (R²≥ 0.98) and no interference was observed. The LOD and LOQ values were between 2.76 µg kg⁻¹ to 53.61 µg kg⁻¹ and 9.19 µg kg⁻¹ to 178.71 µg kg⁻¹, respectively. The recovery, repeatability RDS_r and reproducibility RDS_R values of compounds were calculated between 93.7–109.2%, 1–15%, and 1–13%, respectively. Consequently, results obtained with the evaluation of all parameters were found to be compatible with the SANTE validation criteria, so the method was reliable, effective and easy to use for the detection of insecticides and metabolites in maize silage with LC MS/MS.

Keywords:

• Insecticides
• LC-MS/MS
• maize silage
• multiresidue
• metabolites

Acknowledgments

It is a part of İsmail AZAR’s Ph.D thesis studies in the Graduate School of Natural and Applied Science of Bursa Uludag University and does not require ethics committee approval. There were no conflicts of interest regarding this research. Nabi Alper KUMRAL and İsmail AZAR designed and set up the experiments, İsmail AZAR performed all of the tests, contributed in writing, reading, and approving the manuscript. The authors thanks to İsmail FİLYA, Aysegul YILDIRIM KUMRAL and Mustafa YAVUZ for editorial and technical assistance.

Data Availability Statement

Raw data were generated at Central Research Institute of Food and Feed Control. The data that support the findings of this study are available at [https://drive.google.com/drive/folders/10E-soIpW1tX3CqLGYhvrCsbfON4EOnOC?usp=sharing]. Derived data supporting the findings of this study are available from the corresponding author [İ.A.] on request.

Additional information

Funding

The study was funded by TAGEM (Project grant no. TAGEM/HSGYAD/A/19/A3/P1/1250).