Multiresidue analysis of beta-agonists in bovine and porcine urine, feed and hair using liquid chromatography electrospray ionisation tandem mass spectrometry

Abstract

The use of beta-agonists as growth promoters in cattle breeding is forbidden in many countries for reasons of fair trade and consumer protection. In recent years the use of liquid chromatography (LC) tandem mass spectrometry (MS/MS) has been shown to be the method of choice for the control of beta-agonists. In this study an LC-MS/MS multiresidue analysis method is presented for trace analysis of 22 beta-agonists. A truly generic concept has been designed based on mixed-mode solid-phase extraction and positive electrospray ionisation LC-MS/MS operated in the multiple reaction monitoring mode. This method allows application to a wide variety of sample matrices such as urine, feed and hair, following minor modifications to the analysis procedure only. The method features fit-for-purpose sensitivity in urine as shown by CCalpha and CCbeta values of less than 0.2 and less than 0.5 microg/l respectively, for all beta-agonists studied (terbutaline and reproterol, less than 0.3 and less than 1.0 respectively). Similar but semiquantitative application to feed and hair showed CCbeta values of less than 10.0 and less than 5.0 microg/kg, respectively. A further simplification and improvement is demonstrated using Ultra Performance LC (UPLC) and fast-switching MS/MS. The successful validation of this method following the latest EU requirements and its application to real samples demonstrate that a new versatile tool has been achieved for veterinary control of beta-agonists.

Determination of Ractopamine Residues in Pigs by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

“…Studies of ractopamine residue detection after different treatment schedules in different animal species have been reported by several authors (Elliot et al, 1998;Qiang et al, 2007;Smith & Shelver, 2002;Thompson et al, 2008). Published studies report on tissue residues of ractopamine and its urinary excretion (Antignac et al, 2002;Blanca et al, 2005;Dickson et al, 2005;Moragues & Igualada, 2009;Nielen et al, 2008;Thompson et al, 2008;Van Hoof et al, 2005) and ractopamine residues in hair (Nielen et al, 2008). However, there are little data on the accumulation of ractopamine in pig hair (white or black) as a novel matrix for the control of ractopamine illegal use.…”

Full-scan accurate mass selectivity of ultra-performance liquid chromatography combined with time-of-flight and orbitrap mass spectrometry in hormone and veterinary drug residue analysis

“…The two-stage mass selection provides the selectivity and sensitivity to enable the detection, identification, and quantification of preselected targets at low ng/g level in complex biological matrices such as urine, feces, tissue, feed, and hair [1]. The recent introduction of ultra-performance (UP)LC and fast-switching QqQ-MS/MS instruments significantly increased the number of targets that can be detected in one analysis [2]. However, analytes might move out from the acquired MRM time windows.…”

Optical biosensors for food quality and safety assurance—a review

“…The use of β-agonists as growth promoters have harmful effects and their detection is generally done using liquid chromatography and mass spectrometry (Nielen et al 2008). A novel method for the simultaneous determination of β 2 -agonist residues such as terbutaline, salbutamol, and clenbuterol by high-performance liquid chromatography (HPLC) coupled with chemiluminescence (CL) detection in pig liver samples gave the limits of detection at a signal-tonoise ratio of 3 ranged from 0.007 to 0.01 ng/g and the limits of quantification at a signal-to-noise ratio of 10 ranged from 0.023 to 0.033 ng/g for three β 2 -agonists (Zhang et al 2007).…”