ISSN print edition: 0366-6352 ISSN electronic edition: 1336-9075 Registr. No.: MK SR 9/7 Published monthly

Development of a GREEN analytical technique for detecting sulfamethoxypyridazine in soil and water by QuEChERS/SPE-ESI-LC/MS/MS

Atanu Sarkar, Suman Gupta, Tirthankar Banerjee, K. M. Manjaiah, and Neethu Narayanan

Division of Agricultural Chemicals, ICAR-Indian Agricultural Research Institute, New Delhi, India

E-mail: neethu853@gmail.com

Received: 3 December 2023  Accepted: 18 May 2024

Abstract:

Antibiotics are widely used as drugs to promote growth of livestock as well as to protect humans, fish, cattle, crops, and other living things from microbial infections. Significant amounts of antibiotic residues have been found in soil, edible parts of crops, manures made of animal excreta as well as in wastewater and this causes the rise of a serious problem of antibiotic resistance development. In this study, we have developed a GREEN extraction method for sulfamethoxypyridazine (SMXP), a sulfonamide veterinary antibiotic, from both soil and water for analysis using LC–MS/MS. An LC–MS/MS method has been optimized with a total run time of 5 min. For the extraction of SMXP from the soil a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe), technique was developed with an acceptable recovery of 102.91–111.26% with a method limit of Quantification (MLOQ) of 0.05 mg/kg and method limit of detection (MLOD) of 0.01 mg/kg. For the extraction of SMXP from water, solid-phase extraction (SPE) using a Hydrophilic Lipophilic Balance (HLB) cartridge was optimized with a recovery of 84–110%. The methods were repeatable as well as reproducible with a relative standard deviation (RSD) of ≤ 10%. The MLOQs were 0.01 and 0.05 mg/L(Kg) at 10:1 signal-to-noise ratio, respectively for water and soil. The developed methods were validated using other sulfonamide antibiotics for extraction from soil and water, and they were found to be acceptable. The sulfonamides exhibited soft matrix effects except for sulfadiazine in soil. To evaluate environmental and occupational hazards associated with the analytical method, an Analytical GREENness score was calculated and its values were 0.52 and 0.64 for the QuEChERS and HLB-SPE methods, respectively, indicating the greener nature of the SPE method. Further, the BAGI metric tool demonstrated values of 75 and 70 for soil and water extraction techniques indicating the applicability of the environmentally and occupationally safe methods. Hence, these methods can be safely used to extract and analyze SMXP and other sulfonamide antibiotics.

Keywords: Extraction; GREEN method; Hydrophilic lipophilic balance cartridges; Solid phase extraction; Sulfonamides; QuEChERS

Full paper is available at www.springerlink.com.

DOI: 10.1007/s11696-024-03529-9

Chemical Papers 78 (10) 6115–6126 (2024)