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
PY - 2016/12/1
Y1 - 2016/12/1
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
SN - 1615-9306
VL - 39
SP - 4794
EP - 4804
JO - Journal of Separation Science
JF - Journal of Separation Science
IS - 24
ER -