Determination of tetracyclines in bovine kidney by liquid chromatography/tandem mass spectrometry with on-line extraction and clean-up

Abstract

A novel, sensitive, high performance liquid chromatography/tandem mass spectrometric (i.e. mass spectrometry/mass spectrometry) method with on-line extraction and clean-up for the screening and confirmation of residues of tetracyclines in kidney has been developed. After liquid extraction of homogenised kidney with McIlvain buffer, an aliquot of the extract is directly injected on the LC/MS/MS system with further extraction and clean-up of the sample on-line. Detection of the analytes was achieved by positive electrospray ionization followed by multiple reaction monitoring. For each tetracycline the collisional decomposition of the protonated molecule to a unique, abundant fragment ion was monitored. The method has been validated for tetracycline, oxytetracycline, chlortetracycline and doxycycline. Calibration curves resulting from spiked blank kidney samples at the 100-1200 microgram/kg level showed good linear correlation. At the level of 600 microgram/kg both within- and between-day precision, as measured by relative standard deviation (RSD), were less than 7%. The limits of detection (LODs) for tetracycline, oxytetracycline, chlortetracycline and doxycyline were 18, 23, 24 and 21 microgram/kg, respectively. The limits of quantification (LOQs) for tetracycline, oxytetracycline, chlortetracycline and doxycyline were 36, 46, 47 and 42 microgram/kg, respectively. The recoveries ranged from 71 to 91%. The procedure provides a rapid, reliable and sensitive method for the determination of residues of tetracyclines in bovine kidney. The advantage of this method over existing methods is its decreased sample preparation and analysis time, which makes the method more suitable for routine analysis.

Restricted access materials and large particle supports for on-line sample preparation: an attractive approach for biological fluids analysis

“…Fast and sensitive analytical methods based on the use of an extraction support coupled to MS were developed for the determination of drugs and metabolites in biofluids [17,42,[159][160][161][162][163][164][165].…”

Analysis of veterinary drug residues in shrimp: A multi-class method by liquid chromatography–quadrupole ion trap mass spectrometry

“…Over the past years liquid chromatography-mass spectrometry (LC-MS) multi-residue methods have been developed for drug groups, such as sulfonamides [8,9], tetracyclines [10,11], quinolones [12], ␤-lactams [13], aminoglycosides [14], cephapirin [15], and cationic dyes [16]. However, multi-class residue methods are relatively scarce, compared to multi-matrix, single-class residues methods.…”

Determination of eight sulfonamides in bovine kidney by liquid chromatography/tandem mass spectrometry with on-line extraction and sample clean-up

“…23 The on-line extraction and clean-up procedure of the crude kidney extract resulted in a very short sample preparation time and high sample throughput with acceptable recoveries making the method very suitable for routine analysis. The aim of this study was to investigate if the LC/MS/MS method could be adapted for the determination of residues of sulfonamides in kidney.…”

“…23 Kidney was extracted with McIlvain buffer and the extract was injected directly for analysis by LC/MS/MS with further extraction and sample clean-up on-line. This resulted in a very short analysis time which made the method very suitable for routine analysis.…”