TY - JOUR

T1 - Mycoestrogen determination in cow milk

T2 - Magnetic solid-phase extraction followed by liquid chromatography and tandem mass spectrometry analysis

AU - Capriotti, Anna Laura

AU - Cavaliere, Chiara

AU - Foglia, Patrizia

AU - La Barbera, Giorgia

AU - Samperi, Roberto

AU - Ventura, Salvatore

AU - Laganà, Aldo

N1 - (Ekstern)

PY - 2016

Y1 - 2016

N2 - Recently, magnetic solid-phase extraction has gained interest because it presents various operational advantages over classical solid-phase extraction. Furthermore, magnetic nanoparticles are easy to prepare, and various materials can be used in their synthesis. In the literature, there are only few studies on the determination of mycoestrogens in milk, although their carryover in milk has occurred. In this work, we wanted to develop the first (to the best of our knowledge) magnetic solid-phase extraction protocol for six mycoestrogens from milk, followed by liquid chromatography and tandem mass spectrometry analysis. Magnetic graphitized carbon black was chosen as the adsorbent, as this carbonaceous material, which is very different from the most diffuse graphene and carbon nanotubes, had already shown selectivity towards estrogenic compounds in milk. The graphitized carbon black was decorated with Fe 3 O 4 , which was confirmed by the characterization analyses. A milk deproteinization step was avoided, using only a suitable dilution in phosphate buffer as sample pretreatment. The overall process efficiency ranged between 52 and 102%, whereas the matrix effect considered as signal suppression was below 33% for all the analytes even at the lowest spiking level. The obtained method limits of quantification were below those of other published methods that employ classical solid-phase extraction protocols.

AB - Recently, magnetic solid-phase extraction has gained interest because it presents various operational advantages over classical solid-phase extraction. Furthermore, magnetic nanoparticles are easy to prepare, and various materials can be used in their synthesis. In the literature, there are only few studies on the determination of mycoestrogens in milk, although their carryover in milk has occurred. In this work, we wanted to develop the first (to the best of our knowledge) magnetic solid-phase extraction protocol for six mycoestrogens from milk, followed by liquid chromatography and tandem mass spectrometry analysis. Magnetic graphitized carbon black was chosen as the adsorbent, as this carbonaceous material, which is very different from the most diffuse graphene and carbon nanotubes, had already shown selectivity towards estrogenic compounds in milk. The graphitized carbon black was decorated with Fe 3 O 4 , which was confirmed by the characterization analyses. A milk deproteinization step was avoided, using only a suitable dilution in phosphate buffer as sample pretreatment. The overall process efficiency ranged between 52 and 102%, whereas the matrix effect considered as signal suppression was below 33% for all the analytes even at the lowest spiking level. The obtained method limits of quantification were below those of other published methods that employ classical solid-phase extraction protocols.

KW - Dispersive solid-phase extraction

KW - Graphitized carbon black

KW - Magnetic nanoparticles

KW - Mycoestrogens

KW - Resorcylic acid lactones

UR - http://www.scopus.com/inward/record.url?scp=85005808143&partnerID=8YFLogxK

U2 - 10.1002/jssc.201600879

DO - 10.1002/jssc.201600879

M3 - Journal article

C2 - 27774728

AN - SCOPUS:85005808143

VL - 39

SP - 4794

EP - 4804

JO - HRC & CC, Journal of High Resolution Chromatography and Chromatography Communications

JF - HRC & CC, Journal of High Resolution Chromatography and Chromatography Communications

SN - 1615-9306

IS - 24

ER -