Ionic liquid-based dispersive liquid-liquid microextraction of anthelmintic drug residues in small-stock meat followed by LC-ESI-MS/MS detection

Rebagamang Tshepho; Simiso Dube; Mathew M Nindi

doi:10.1002/fsn3.3568

Ionic liquid-based dispersive liquid-liquid microextraction of anthelmintic drug residues in small-stock meat followed by LC-ESI-MS/MS detection

Food Sci Nutr. 2023 Jul 22;11(10):6288-6302. doi: 10.1002/fsn3.3568. eCollection 2023 Oct.

Authors

Rebagamang Tshepho^{1

2}, Simiso Dube¹, Mathew M Nindi³

Affiliations

¹ Department of Chemistry, College of Science, Engineering and Technology, The Science Campus University of South Africa Roodepoort, Johannesburg South Africa.
² Residue Section Botswana National Veterinary Laboratory Gaborone Botswana.
³ Institute for Nanotechnology and Water Sustainability (iNanoWS), The Science Campus, College of Science, Engineering and Technology (CSET) University of South Africa Roodepoort, Johannesburg South Africa.

Abstract

An ionic liquid-based dispersive liquid-liquid microextraction (IL-DLLME) of 20 anthelmintic drugs followed and detected by liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed, optimized, and validated. The parameters affecting the anthelmintic extraction efficiencies such as selection of extraction solvent (ionic liquids), selection of disperser solvent, volume of extraction solvent, volume of disperser solvent, pH of the aqueous phase, extraction time, salt addition, and centrifugation time were optimized. Validation was conducted according to ISO/IEC 17025:2017 and Commission Implementing Regulation (EU) 2021/808 of 22 March 2021. Validation parameters such as calibration function, matrix effect, limit of detection (LOD), limit of quantification (LOQ), decision limit (CCα), accuracy, and precision were established. Coefficient of determination (R ²) values ranging from .99938 to .99995 were obtained using the matrix calibration curve spiked at 0, 0.25, 1.0, 1.5, and 2.0 times MRL. The LODs and LOQs were calculated using the standard deviation of the response and the slopes of the calibration curves ranged from 0.35 to 26.1 μg/kg and from 1.2 to 87.0 μg/kg, respectively, and were dependent on calibration range. The CCα values ranged from 23 to 1022.0 μg/kg and are also dependent on the MRL concentration levels. The coefficient of variation (CV) values calculated are within the reproducibility range of 16%-30% adapted from the Horwitz Equation CV = 2^{(1-0.5 log C)} and ranged from 1.7% to 16.9%. The developed and validated and the standard QuEChERS method were compared. The IL-DLLME LC-MS/MS method was applied to 32 small stock (18 caprine [goat] and 14 ovine [sheep]) liver samples received from municipal abattoirs at Botswana National Veterinary Laboratory for the analysis of anthelmintic drug residues. The results obtained indicated that the anthelmintic drug residues were all below the detection capability, and therefore, the samples were passed as fit for human consumption.

Keywords: anthelmintic drugs; caprine; green sample preparation; ionic liquid‐dispersive liquid–liquid microextraction; ovine.