Towards high throughput analysis using 96-well plate solid phase extraction to determine sedatives and β-blocker residues in food control monitoring

• Published in: Analytica chimica acta Vol. 1331; p. 343335
• Main Authors: Arrizabalaga-Larrañaga, Ane, van Doorn, Dieke, Sterk, Saskia S.
• Format: Journal Article
• Language: English
• Published: Elsevier B.V 01-12-2024
• Subjects: Animal tissues; Food safety; LC-MS/MS; Sample preparation; Sedatives; Sedatives; LC-MS/MS; Food safety; Sample preparation; Animal tissues
• ISSN: 0003-2670; 1873-4324; 1873-4324
• DOI: 10.1016/j.aca.2024.343335

Veterinary drugs are widely used in animal production to prevent infections and treat diseases but, this may cause a risk to consumers. Due to the high number of food samples required to monitor yearly, simple, fast, sensitive and selective analytical methods are needed in control laboratories to ensure consumers safety. Nevertheless, many analytical methodologies available in these laboratories include multiple steps and therefore are time-consuming and hinder the analysis throughput requiring significant amounts of solvents and reagents.
This work developed a 96-well plate solid phase extraction (SPE) method for the extraction of seven sedatives and a β-blocker in animal kidney by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC−MS/MS). The developed method was validated based on Implementing Regulation (EU) 2021/808 in kidney, meat and fish. The performance characteristics of the validation (1–5 μg kg−1) showed good linearity (R2 > 0.998) while decision limits (CCα) were between 1 and 1.2 μg kg−1. Trueness and precision were determined at three levels (n = 7) and the results showed values ranging from 85 to 103 % and from 1 to 9 %, respectively. The feasibility of the method was demonstrated for the residue control requirement established by EU. Method was applied to 201 samples of kidney, meat and fish.
This study is the first to present an optimized and validated holistic method for sedatives and β-blocker using 96-well plate SPE and UHPLC−MS/MS. The method showed good performance in kidney, meat and fish samples being an universal method for any species along the same type of sample. The fast, easy, efficient, reliable and universal method showed high throughput and so reduced the analysis time by nine-fold and the required solvent amount by four times fulfilling the green chemistry principals.
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•Validated SPE method for kidney analysis of sedatives and β-blocker was developed.•Single matrix fortified calibration curve to quantify different animal species.•The developed method has been successfully extended to meat and fish samples.•96-well plate format permit future automation of sample preparation.•Method is implemented in the National Control Monitoring Plan for food residues.