2.5. LC–MS/MS analysis of olive phenols
The samples were analysed by electro spray ionization tandem
mass spectrometry (ESI-MS/MS) using a MSD Sciex Applied Biosystem
API 4000 Q-Trap mass spectrometer. The LC–MS was operated
in the negative ion mode using multiple reaction monitoring
(MRM). The experimental conditions were as follow: ionspray voltage
(IS) 4500 V; curtain gas 20 psi; temperature 400 C; ion
source gas(1) 35 psi; ion source gas(2) 45 psi; collision gas thickness
(CAD) medium; entrance potential (EP), declustering potential
(DP), entrance collision energy (CE) and exit collision energy (CXP)
were optimized for each transition monitored.
The analytes were separated on an Eclipse XDB-C8-A HPLC column
[(5 lm particle size, 50 mm length and 4.6 mm i.d.) (Agilent
Technologies, Santa Clara, California)] at a flow rate of
350 lL min1 with an injection volume of 10 lL. A binary mobile
phase made up of 0.1% aqueous formic acid (A) and methanol (B)
was gradient programmed to increase B from 10% to 100% in
10 min, hold for 2 min and ramp down to original composition
(90% A and 10% B) in eight minutes. The total elution time was
20 min per injection.
2.5. LC–MS/MS analysis of olive phenolsThe samples were analysed by electro spray ionization tandemmass spectrometry (ESI-MS/MS) using a MSD Sciex Applied BiosystemAPI 4000 Q-Trap mass spectrometer. The LC–MS was operatedin the negative ion mode using multiple reaction monitoring(MRM). The experimental conditions were as follow: ionspray voltage(IS) 4500 V; curtain gas 20 psi; temperature 400 C; ionsource gas(1) 35 psi; ion source gas(2) 45 psi; collision gas thickness(CAD) medium; entrance potential (EP), declustering potential(DP), entrance collision energy (CE) and exit collision energy (CXP)were optimized for each transition monitored.The analytes were separated on an Eclipse XDB-C8-A HPLC column[(5 lm particle size, 50 mm length and 4.6 mm i.d.) (AgilentTechnologies, Santa Clara, California)] at a flow rate of350 lL min1 with an injection volume of 10 lL. A binary mobilephase made up of 0.1% aqueous formic acid (A) and methanol (B)was gradient programmed to increase B from 10% to 100% in10 min, hold for 2 min and ramp down to original composition(90% A and 10% B) in eight minutes. The total elution time was20 min per injection.
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