LC-MS/MS Determination of 21 Non-Steroidal Anti-Inflammatory Drugs Residues in Animal Milk and Muscles.

Marta Pietruk,Piotr Jedziniak,Małgorzata Olejnik

doi:10.3390/molecules26195892

Abstract

The presented procedure combines experience from two LC-MS/MS methods previously developed by our team for NSAIDs determination in meat and milk. The novelty was a modification of sample preparation and combining LC-MS/MS method for milk and muscle. The clean-up procedure was investigated, leading to a change from SPE to dSPE with C18 bulk sorbent. Unlike most of the existing methods, chromatographic separation was achieved on a C8 chromatographic column. This method was developed and validated under European Commission Decision 2002/657/EC. Recovery for milk samples values between 86.3% to 108%, with the coefficient of variation, varied from 5.51% to 16.2%. The recovery for muscle was calculated to be between 85.0% and 109%, and the coefficient of variation was—4.73% to 16.6%. The validation results prove that the method is suitable for confirmatory purposes in milk and muscle. Of 452 samples tested in 2019 and 2020, two have been identified as non-compliant.

Highlights

Non-steroidal anti-inflammatory drugs (NSAIDs) are commonly used pharmaceuticals in both human and animal medicine
NSAIDs are a group of polar compounds; the electrospray ionisation (ESI) source is the most suitable choice
It was previously established that the negative ionisation is suitable for more acidic NSAIDs, and positive ionisation showed better results for metamizole metabolites, some coxibs, and NSAIDs [18]

Summary

Introduction

Non-steroidal anti-inflammatory drugs (NSAIDs) are commonly used pharmaceuticals in both human and animal medicine. They can reduce pain, inflammation, prevent blood clots, and decrease fever. Despite the similar mechanism of action (inhibition of the enzymes responsible for proteinoid synthesis—COX), NSAIDs are a diverse group of drugs, with different half-lives, from 4 h for ibuprofen, diclofenac or acetaminophen, to 20–60 h for oxicams (in human) [2]. In veterinary medicine, they became an essential class of medications for most mammalian animals. Recent findings show NSAIDs residues can cause deadly threats for many animal species, such as Indian vultures who die due to diclofenac poisoning [5]

Objectives

Methods

Results