A new analytical method that uses high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) was developed for the first time for the analysis of vitamins B2 (riboflavin) and B3 (nicotinamide and nicotinic acid) in anchovies. Samples were extracted using four different extraction procedures: acidic hydrolysis (method 1), acidic hydrolysis plus peptide precipitation (method 2), acidic plus enzymatic hydrolysis (method 3) and enzymatic hydrolysis (method 4), and method 1 was found to be very good in terms of recoveries and quantitative results. From an analytical point of view, the separation of three analytes was achieved using a Kinetex Hilic analytical column (100 mm × 4.6 mm i.d.) with isocratic elution in a very short time (2.5 min or chromatography run). The recovery percentages (for method 1) obtained by spiking the matrices at 2.5 and 20 mg kg−1 with a standard mixture of the three analytes were in the range 96.2-105.3%; the correlation coefficients (R2) were always higher than 0.9996, and limits of quantification (LOQs) for all compounds were in the range 1–5 μg kg−1. Once validated, method 1 was applied to the analysis of 28 anchovy samples, both fresh and canned ones.
Optimization of an extraction procedure for the simultaneous quantification of riboflavin, nicotinamide and nicotinic acid in anchovies (Engraulis enrasicolus) by high-performance liquid chromatography–tandem mass spectrometry
Giovanni Caprioli;Gianni Sagratini;Sauro Vittori;Elisabetta Torregiani
2018-01-01
Abstract
A new analytical method that uses high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) was developed for the first time for the analysis of vitamins B2 (riboflavin) and B3 (nicotinamide and nicotinic acid) in anchovies. Samples were extracted using four different extraction procedures: acidic hydrolysis (method 1), acidic hydrolysis plus peptide precipitation (method 2), acidic plus enzymatic hydrolysis (method 3) and enzymatic hydrolysis (method 4), and method 1 was found to be very good in terms of recoveries and quantitative results. From an analytical point of view, the separation of three analytes was achieved using a Kinetex Hilic analytical column (100 mm × 4.6 mm i.d.) with isocratic elution in a very short time (2.5 min or chromatography run). The recovery percentages (for method 1) obtained by spiking the matrices at 2.5 and 20 mg kg−1 with a standard mixture of the three analytes were in the range 96.2-105.3%; the correlation coefficients (R2) were always higher than 0.9996, and limits of quantification (LOQs) for all compounds were in the range 1–5 μg kg−1. Once validated, method 1 was applied to the analysis of 28 anchovy samples, both fresh and canned ones.File | Dimensione | Formato | |
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