TY - JOUR
T1 - Injection-port derivatization coupled to GC-MS/MS for the analysis of glycosylated and non-glycosylated polyphenols in fruit samples
AU - Marsol-Vall, Alexis
AU - Balcells, Mercè
AU - Eras, Jordi
AU - Canela-Garayoa, Ramon
N1 - Publisher Copyright:
© 2016 Elsevier Ltd. All Rights Reserved.
PY - 2016/8/1
Y1 - 2016/8/1
N2 - Polyphenols, including glycosylated polyphenols, were analyzed via a procedure based on injection-port derivatization coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS). The polyphenols in lyophilized fruit samples were extracted with an acidified MeOH mixture assisted by ultrasound. Samples were dried under vacuum, and carbonyl groups were protected with methoxylamine. Free hydroxyl groups were subsequently silylated in-port. Mass fragmentations of 17 polyphenol and glycosylated polyphenol standards were examined using Multiple Reaction Monitoring (MRM) as the acquisition mode. Furthermore, in-port derivatization was optimized in terms of optimal injection port temperature, derivatization time and sample: N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) volume ratio. A C18 solid-phase-extraction clean-up method was used to reduce matrix effects and injection liner degradation. Using this clean-up method, recoveries for samples spiked at 1 and 10 μg/g ranged from 52% to 98%, depending on the chemical compound. Finally, the method was applied to real fruit samples containing the target compounds. The complete chromatographic runtime was 15 min, which is faster than reported for recent HPLC methods able to analyze similar compounds.
AB - Polyphenols, including glycosylated polyphenols, were analyzed via a procedure based on injection-port derivatization coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS). The polyphenols in lyophilized fruit samples were extracted with an acidified MeOH mixture assisted by ultrasound. Samples were dried under vacuum, and carbonyl groups were protected with methoxylamine. Free hydroxyl groups were subsequently silylated in-port. Mass fragmentations of 17 polyphenol and glycosylated polyphenol standards were examined using Multiple Reaction Monitoring (MRM) as the acquisition mode. Furthermore, in-port derivatization was optimized in terms of optimal injection port temperature, derivatization time and sample: N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) volume ratio. A C18 solid-phase-extraction clean-up method was used to reduce matrix effects and injection liner degradation. Using this clean-up method, recoveries for samples spiked at 1 and 10 μg/g ranged from 52% to 98%, depending on the chemical compound. Finally, the method was applied to real fruit samples containing the target compounds. The complete chromatographic runtime was 15 min, which is faster than reported for recent HPLC methods able to analyze similar compounds.
KW - Fruit samples
KW - GC-MS/MS
KW - Glycosylated polyphenols
KW - In-port derivatization
KW - Non-glycosylated polyphenols
UR - http://www.scopus.com/inward/record.url?scp=84959440446&partnerID=8YFLogxK
U2 - 10.1016/j.foodchem.2016.02.089
DO - 10.1016/j.foodchem.2016.02.089
M3 - Article
C2 - 26988495
AN - SCOPUS:84959440446
SN - 0308-8146
VL - 204
SP - 210
EP - 217
JO - Food Chemistry
JF - Food Chemistry
ER -