Volatolomics approach for authentication of not-from-concentrate (NFC) orange juice based on characteristic volatile markers using headspace solid phase microextraction (HS-SPME) combined with GC-MS

Applications of Ultrahigh Performance Liquid Chromatography Electrospray Ionization Q-Orbitrap Mass Spectrometry and QuEChERS for Fingerprinting and Identification of Molecular Markers in Orange Juices

“…Figure D showed one of the compounds that was tentatively identified (Level 2a “Probable structure” identification with literature or unambiguous mass library spectrum-structure matching) as nootkatone in orange juices with the mass spectral matching in mzCloud (see Supporting Information) and a publication (or LC-MS/MS spectrum) . Nootkatone was one of many volatile organic compounds (VOCs) in orange juices. ,− The VOCs in orange juices have been utilized to differentiate NFCs and FCs using headspace solid phase microextraction (HS-SPME) combined with GC-MS . In the current study, it was observed that the amounts of nootkatone and other three compounds chosen (Compound A (C 11 H 14 O), B (C 9 H 10 O), and C (C 8 H 16 O 3 ).…”

“…However, differential analysis allowed differentiation of NFCs and FCs. It has been reported that certain molecules in orange juices may be subjected to change or be lost during their manufacturing procedure through evaporation and concentration, or experience chemical reaction to form new substances by thermal decomposition when preparing orange juice concentrates or reconstituting orange juices from their concentrates. ,, For example, some volatile organic compounds such as ethyl butyrate, methyl hexanoate, 5-methyl-1-heptanol, etc., which were characteristic markers, were present in NFCs but were undetectable in FCs, and other volatile compounds such as α-calacorene, 2-methyl-3-buten-2-ol, were relatively high in amounts in FCs compared to NFCs . The amount of citrus flavonoids, organic acids, and alkaloids was higher in NFCs than in FCs .…”

“…Sample preparation can be as simple as a procedure by centrifugation, filtration, or 1:1 methanol dilution prior to LC injection for orange juice fingerprinting or profiling using UHPLC HRMS. ,, The analysis of volatile organic compounds in orange juices was achieved using headspace solid phase microextraction (HS-SPME) combined with GC-MS. , In the current study, we explored QuEChERS (salting-out acetonitrile/water extraction and partition) without d-SPE cleanup for fingerprinting and identification of markers in orange juices using an UHPLC/ESI Q-Orbitrap. QuEChERS provided relatively clean sample extracts by removing particles, sugar, and relatively polar compounds found in the orange juices, and therefore helped to maintain the performance of the Q-Orbitrap over time in routine applications where a large number of samples were analyzed each day .…”

“…UHPLC-QTOF has been utilized to distinguish the geographic origin and variety of citrus fruit/fruit juice, and detect fruit juices adulterated with other fruit juices down to 1% or 2% and diluted with water down to 5% when comparing to original unadulterated or undiluted orange juices as a reference. , UHPLC QTOF or nontarget metabolomics provided principle component analysis (PCA) score plots that differentiated orange juices made “From Concentrate” (FCs) and “Not From Concentrate” (NFCs), and determined several potential markers which were further used in the discrimination of NFC authentication . GC Q-Orbitrap and orthogonal partial least-squares discriminant analysis (OPLS-DA) were able to differentiate FC and NFC orange juices, and a total of 107 volatile organic compounds (VOCs) in NFC and FC orange juices were identified and 10 VOCs were selected as potential markers to differentiate between NFC and FC orange juices for authentication . The volatolomics approach (the determination of highly semivolatile fractions of molecules) or headspace solid-phase microextraction gas chromatography–mass spectrometry has demonstrated its applicability to discriminate between NFC and FC orange juices. , …”

Latest Improvements and Expanding Applications of Solid-Phase Microextraction

“…A total of 107 VOCs have been identified by GC-Q-Exactive Orbitrap, and 10 VOCs have been preliminarily selected as potential characteristic markers in different juices. The accurate quantification of selected markers has been conducted on GC-MS …”