Abstract

A method for the determination of a wide range residues of anti-inflammatory drugs (16 acidic non-steroidal anti-inflammatory drugs and four metamizole metabolites and five corticosteroids) has been was developed. In the first step of sample preparation, acetate buffer was added to minced muscle samples and 15-min ultrasound-assisted enzymatic hydrolysis was performed. Next, the samples were extracted twice with acetonitrile, freezed and analysed. The analytes were separated on a C18 column with a 25-min gradient of methanol/acetonitrile (8:2) and 0.05 M ammonium formate at pH 5.0 and determined by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was validated according to the requirements described in the Commission Decision 2002/657/EC: linearity, precision (repeatability and within-laboratory reproducibility), accuracy, decision limit CCα and detection capability CCβ were calculated. The method developed fulfilled the performance criteria and can be used in the official control of veterinary drug residues in food of animal origin. The method was positively verified in the proficiency test and in the analysis of incurred material.

Highlights

  • Non-steroidal anti-inflammatory drugs (NSAIDs) and glucocorticosteroids (GCs) are widely used in veterinary medicine as well as in treatment of diseases in food-producing animals

  • In the case of NSAIDs, maximum residue limits (MRLs) values were established in animal muscle for the following: salicylic acid (400 μg kg−1 for turkey), flunixin (10 μg kg−1 for Equidae, 20 μg kg−1 for bovine, 50 μg kg−1 for porcine), meloxicam (20 μg kg−1 for bovine, caprine, porcine, rabbit, Equidae), metamizole, diclofenac (5 μg kg−1 for bovine, porcine), tolfenamic acid (50 μg kg−1 for bovine, porcine), carprofen (500 μg kg−1 for bovine, Equidae) and firocoxib (10 μg kg−1, Equidae)

  • Chrusch et al published the procedure for the simultaneous determination of 29 veterinary drugs (NSAIDs, GCs and anabolic steroids) in animal tissues based on acidic hydrolysis, multistage solid-phase extraction (SPE) clean-up and different LC conditions for specific groups of analytes (Chrusch et al 2008)

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Summary

Introduction

Non-steroidal anti-inflammatory drugs (NSAIDs) and glucocorticosteroids (GCs) are widely used in veterinary medicine as well as in treatment of diseases in food-producing animals. Chrusch et al published the procedure for the simultaneous determination of 29 veterinary drugs (NSAIDs, GCs and anabolic steroids) in animal tissues based on acidic hydrolysis, multistage solid-phase extraction (SPE) clean-up and different LC conditions for specific groups of analytes (Chrusch et al 2008). The authors want to share their experience in the determination of NSAIDs in animal tissues ( Jedziniak et al 2010, Jedziniak et al 2013b, Olejnik et al 2013) and develop a new method with wider range of analytes (both metamizole metabolites and Bacidic^ NSAIDs and GC), enzymatic hydrolysis step and simple sample preparation. According to the best authors’ knowledge, methods for the simultaneous determination of NSAIDs and GCs with enzymatic hydrolysis were not published Such approach ensures faster and cheaper analysis and allows to determine conjugated analytes, what is not possible with previously published procedures

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