Analysis of non-steroidal anti-inflammatory drugs in milk using QuEChERS and liquid chromatography coupled to mass spectrometry: triple quadrupole versus Q-Orbitrap mass analyzers.
We developed a Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method for the high throughput determination of 10 non-steroidal anti-inflammatory drugs (NSAIDs) in milk samples using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) with a triple quadrupole (QqQ) instrument and an electrospray ionization (ESI) source. The new extraction procedure is highly efficient, and we obtained absolute recoveries in the range 78.1-97.1 % for the extraction and clean-up steps. Chromatographic separation is performed in the gradient mode with a biphenyl column and acidic mobile phases consisting of water and acetonitrile containing formic acid. The chromatographic run time was about 12 min, and NSAID peaks showed a good symmetry factor. For MS/MS detection, we used multiple reaction monitoring (MRM) mode, using ESI in both positive and negative modes. Our method has been validated in compliance with the European Commission Decision 657/2002/EC, and we obtained very satisfactory results in inter-laboratory testing. Furthermore, we explored the use of a hybrid high resolution mass spectrometer, combining a quadrupole and an Orbitrap mass analyzer, for high resolution (HR) MS/MS detection of NSAIDs. We achieved lower NSAID quantification limits with Q-Orbitrap high resolution mass spectrometry (HRMS/MS) detection than those achieved with the QqQ instrument; however, its main feature is its very high selectivity, which makes HRMS/MS particularly suitable for confirmatory analysis.
Laboratori de l'Agència de Salut Pública de Barcelona, Avinguda Drassanes 13-15, 08001, Barcelona, Spain. arubies@aspb.cat.
Antoni
A
Rúbies
Laboratori de l'Agència de Salut Pública de Barcelona, Avinguda Drassanes 13-15, 08001, Barcelona, Spain.|Department de Química Analítica, Universitat de Barcelona, Martí Franquès 1-11, 08028, Barcelona, Spain.
Lili
L
Guo
Laboratori de l'Agència de Salut Pública de Barcelona, Avinguda Drassanes 13-15, 08001, Barcelona, Spain.|CIBER of Epidemiology and Public Health (CIBERESP), 28029, Madrid, Spain.
Francesc
F
Centrich
Department de Química Analítica, Universitat de Barcelona, Martí Franquès 1-11, 08028, Barcelona, Spain.
Mercè
M
Granados
D000818:Animals; D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis* / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods; D005506:Food Contamination / Q000032:analysis; D057230:Limit of Detection; D008892:Milk / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*
D000894:Anti-Inflammatory Agents, Non-Steroidal
Liquid chromatography; Mass spectrometry; Milk; Non-steroidal anti-inflammatory drugs; Q-Orbitrap; Triple quadrupole