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
Por:
Rubies, A, Guo, LL, Centrich, F, Granados, M
Publicada:
1 ago 2016
Resumen:
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.
Filiaciones:
Rubies, A:
Lab Agencia Salut Publ Barcelona, Avinguda Drassanes 13-15, Barcelona 08001, Spain
Guo, LL:
Lab Agencia Salut Publ Barcelona, Avinguda Drassanes 13-15, Barcelona 08001, Spain
Univ Barcelona, Dept Quim Analit, Marti Franques 1-11, E-08028 Barcelona, Spain
Centrich, F:
Lab Agencia Salut Publ Barcelona, Avinguda Drassanes 13-15, Barcelona 08001, Spain
CIBER Epidemiol & Publ Hlth CIBERESP, Madrid 28029, Spain
Granados, M:
Univ Barcelona, Dept Quim Analit, Marti Franques 1-11, E-08028 Barcelona, Spain
Green Accepted
|