New method for the analysis of lipophilic marine biotoxins in fresh and canned bivalves by liquid chromatography coupled to high resolution mass spectrometry: a quick, easy, cheap, efficient, rugged, safe approach.

A new method for the analysis of lipophilic marine biotoxins (okadaic acid, dinophysistoxins, azaspiracids, pectenotoxins, yessotoxins, spirolids) in fresh and canned bivalves has been developed. A QuEChERS methodology is applied; i.e. the analytes are extracted with acetonitrile and clean-up of the extracts is performed by dispersive solid phase extraction with C18. The extracts are analyzed by ultra-high performance liquid chromatography coupled to a hybrid quadrupole-Orbitrap mass spectrometer, operating in tandem mass spectrometry mode, with resolution set at 70,000 (m/z 200, FWHM). Separation of the analytes, which takes about 10min, is carried out in gradient elution mode with a BEH C18 column and mobile phases based on 6.7mM ammonia aqueous solution and acetonitrile mixtures. For each analyte the molecular ion and 1 or 2 product ions are acquired, with a mass accuracy better than 5ppm. The quantification is performed using surrogate matrix matched standards, with eprinomectin as internal standard. The high-throughput method, which has been successfully validated, fulfills the requirements of European Union legislation, and has been implemented as a routine method in a public health laboratory.

Comparison of triple quadrupole mass spectrometry and Orbitrap high-resolution mass spectrometry in ultrahigh performance liquid chromatography for the determination of veterinary drugs in sewage: benefits and drawbacks.

This paper presents a comparison of triple quadrupole tandem mass spectrometry (MS/MS) and Orbitrap high-resolution mass spectrometry (HRMS) combined to ultrahigh performance liquid chromatography for the determination of glucocorticoids and polyether ionophores in sewage, in order to show the major benefits and drawbacks for each mass spectrometry analyser. Overall, HRMS measurements have enhanced performance in terms of confirmatory capabilities than MS/MS measurements. Moreover, similar limits of quantification, limits of detection, linear range and repeatability for glucocorticoids with both the MS/MS and HRMS methods were compared, but in the case of polyether ionophores, slightly better limits of detection and limits of quantification were obtained with the HRMS method because of the high sensitivity obtained when diagnostic ions are used for quantification instead of selected reaction monitoring transitions for these compounds. The two methods have been applied to the analysis of several influent and effluent sewage samples from sewage treatment plants located in the Tarragona region (Catalonia, Spain), showing an excellent correlation between the two methods.