Development of fast screening methods for the analysis of veterinary drug residues in milk by liquid chromatography-triple quadrupole mass spectrometry

• Published in: Analytical & bioanalytical chemistry (Print) Vol. 397; no. 7; pp. 2777 - 2790
• Main Authors: Martínez Vidal, José Luis, Frenich, Antonia Garrido, Aguilera-Luiz, María M., Romero-González, Roberto
• Format: Journal Article Conference Proceeding
• Language: English
• Published: Berlin/Heidelberg Springer-Verlag 01.08.2010; Springer
• Subjects: Analytical Chemistry; Animals; Biochemistry; Cattle; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - methods; Comparative analysis; Drug Residues - analysis; Drugs; Exact sciences and technology; Food Contamination - analysis; Food Science; High performance liquid chromatography; Laboratory Medicine; Liquids; Mass spectrometry; Mathematical analysis; Methods; Milk; Milk - chemistry; Monitoring/Environmental Analysis; Original Paper; Other chromatographic methods; Quadrupoles; Residues; Screening; Spectrometric and optical methods; Tandem Mass Spectrometry - methods; Veterinary; Veterinary Drugs - analysis; Triple quadrupole; UHPLC; Veterinary drugs; Screening methods; Milk; Triple quadrupole UHPLC; Chemical analysis; Choice; Selection; HPLC chromatography; Product; Identification; Time; Quadrupole spectrometer; Target; Sample preparation; False negative; Extraction; Time analysis; Monitoring; Quantitative analysis; Trace analysis; Drug; Sample; Liquid chromatography; Screening; Analysis method; Residue; Mass spectrometry MS/MS; Analytical method; Reference material; Mass spectrometry
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-009-3425-1

Two rapid multi-residue screening methods for the determination of 21 veterinary drugs in milk by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) have been developed and compared. For both methods, veterinary drugs were extracted from milk samples using a rapid extraction procedure based on the modification of the well-known QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method, and no further clean-up steps were necessary. One screening method was based on the selection of a characteristic neutral loss or product ion of the various families of compounds, whereas another one was based on the choice of a selected reaction monitoring (SRM) for each compound. These methods were compared with regards to false negatives, cut-off values and the unreliability region. The total run time for both methods was 3 min, allowing quick selection of samples that contained veterinary drugs. Non-negative samples were re-analyzed by the UHPLC-MS/MS confirmation/quantification method, which consisted in the monitoring of two SRM for each compound. The methods were validated according to international guides. The proposed analytical methods allow for the identification and confirmation of the target veterinary drugs at trace levels employing quick analysis time.