Summary of Study ST003708

This data is available at the NIH Common Fund's National Metabolomics Data Repository (NMDR) website, the Metabolomics Workbench, https://www.metabolomicsworkbench.org, where it has been assigned Project ID PR002302. The data can be accessed directly via it's Project DOI: 10.21228/M82R84 This work is supported by NIH grant, U2C- DK119886.

See: https://www.metabolomicsworkbench.org/about/howtocite.php

This study contains a large results data set and is not available in the mwTab file. It is only available for download via FTP as data file(s) here.

Show all samples | Perform analysis on untargeted data
Download mwTab file (text) | Download mwTab file(JSON) | Download data files (Contains raw data)

Study ID	ST003708
Study Title	Phytochemical analysis of Quercus ilex nuts revealed high variability, nutritional and nutraceutical value.
Study Type	Untargeted metabolomics
Study Summary	In recent years, new feeding systems based on non-conventional crops have been gaining in popularity. Holm oak is a non-domesticated forest species and very dominant in the Mediterranean Basin. Its fruit, the acorn, is under study due to its high nutritional and nutraceutical value. However, the Quercus ilex species presents a great natural variability, producing fruits with very different qualities. Therefore, in this work, 14 individuals distributed in different locations have been selected to characterise their metabolomic profile and to identify bioactive compounds of interest in different industries and compounds that have been previously associated with specific flavours. The acorns have not been previously classified as there are no specialised tasters. The results obtained may be of great value in laying the foundations for the nutritional potential of acorns and may be complemented by other chemical analyses and future studies looking for bittersweet acorns.
Institute	University of Cordoba
Department	Department of Biochemistry and Molecular Biology
Laboratory	AGR-164
Last Name	Tienda
First Name	Marta
Address	Campus de Rabanales, Edificio C6 Severo Ochoa, Ctra. Madrid, Km 396. 14071 Córdoba, Spain
Email	b72tipam@uco.es
Phone	+34 634925272
Submit Date	2025-02-02
Raw Data Available	Yes
Raw Data File Type(s)	mzXML
Analysis Type Detail	Other
Release Date	2025-02-24
Release Version	1

Select appropriate tab below to view additional metadata details:

Project:

Project ID:	PR002302
Project DOI:	doi: 10.21228/M82R84
Project Title:	Phytochemical analysis of Quercus ilex nuts revealed high variability, nutritional and nutraceutical value.
Project Type:	Untargeted Metabolomics Analysis
Project Summary:	14 acorn flours from different individuals of holm oak have been analysed to characterise the variability of the phytochemical profile of the fruit.
Institute:	University of Cordoba
Department:	Department of Biochemistry and Molecular Biology
Laboratory:	AGR-164
Last Name:	Tienda
First Name:	Marta
Address:	Campus de Rabanales, Edificio C6 Severo Ochoa, Ctra. Madrid, Km 396. 14071 Córdoba, Spain
Email:	b72tipam@uco.es
Phone:	+34 634925272

Subject:

Subject ID:	SU003840
Subject Type:	Plant
Subject Species:	Quercus ilex
Taxonomy ID:	58334

Factors:

Subject type: Plant; Subject species: Quercus ilex (Factor headings shown in green)

mb_sample_id	local_sample_id	Sample source	Factor
SA405952	Individual1-rep1_pos_TOP5	Fruit_flour	Individual_1
SA405953	Individual1-rep3_neg_TOP5	Fruit_flour	Individual_1
SA405954	Individual1-rep3_neg	Fruit_flour	Individual_1
SA405955	Individual1-rep2_neg_TOP5	Fruit_flour	Individual_1
SA405956	Individual1-rep2_neg	Fruit_flour	Individual_1
SA405957	Individual1-rep1_neg_TOP5	Fruit_flour	Individual_1
SA405958	Individual1-rep1_pos	Fruit_flour	Individual_1
SA405959	Individual1-rep1_neg	Fruit_flour	Individual_1
SA405960	Individual1-rep3_pos_TOP5	Fruit_flour	Individual_1
SA405961	Individual1-rep2_pos	Fruit_flour	Individual_1
SA405962	Individual1-rep3_pos	Fruit_flour	Individual_1
SA405963	Individual1-rep2_pos_TOP5	Fruit_flour	Individual_1
SA405964	Individual10-rep3_pos_TOP5	Fruit_flour	Individual_10
SA405965	Individual10-rep2_neg_TOP5	Fruit_flour	Individual_10
SA405966	Individual10-rep3_neg_TOP5	Fruit_flour	Individual_10
SA405967	Individual10-rep2_neg	Fruit_flour	Individual_10
SA405968	Individual10-rep1_neg_TOP5	Fruit_flour	Individual_10
SA405969	Individual10-rep1_neg	Fruit_flour	Individual_10
SA405970	Individual10-rep3_neg	Fruit_flour	Individual_10
SA405971	Individual10-rep1_pos	Fruit_flour	Individual_10
SA405972	Individual10-rep1_pos_TOP5	Fruit_flour	Individual_10
SA405973	Individual10-rep2_pos	Fruit_flour	Individual_10
SA405974	Individual10-rep2_pos_TOP5	Fruit_flour	Individual_10
SA405975	Individual10-rep3_pos	Fruit_flour	Individual_10
SA405976	Individual11-rep1_neg	Fruit_flour	Individual_11
SA405977	Individual11-rep1_neg_TOP5	Fruit_flour	Individual_11
SA405978	Individual11-rep2_neg_TOP5	Fruit_flour	Individual_11
SA405979	Individual11-rep3_neg	Fruit_flour	Individual_11
SA405980	Individual11-rep3_pos_TOP5	Fruit_flour	Individual_11
SA405981	Individual11-rep3_pos	Fruit_flour	Individual_11
SA405982	Individual11-rep2_pos	Fruit_flour	Individual_11
SA405983	Individual11-rep1_pos_TOP5	Fruit_flour	Individual_11
SA405984	Individual11-rep1_pos	Fruit_flour	Individual_11
SA405985	Individual11-rep3_neg_TOP5	Fruit_flour	Individual_11
SA405986	Individual11-rep2_neg	Fruit_flour	Individual_11
SA405987	Individual11-rep2_pos_TOP5	Fruit_flour	Individual_11
SA405988	Individual12-rep1_neg_TOP5	Fruit_flour	Individual_12
SA405989	Individual12-rep1_pos_TOP5	Fruit_flour	Individual_12
SA405990	Individual12-rep2_pos	Fruit_flour	Individual_12
SA405991	Individual12-rep2_pos_TOP5	Fruit_flour	Individual_12
SA405992	Individual12-rep3_pos	Fruit_flour	Individual_12
SA405993	Individual12-rep3_pos_TOP5	Fruit_flour	Individual_12
SA405994	Individual12-rep1_neg	Fruit_flour	Individual_12
SA405995	Individual12-rep3_neg_TOP5	Fruit_flour	Individual_12
SA405996	Individual12-rep2_neg	Fruit_flour	Individual_12
SA405997	Individual12-rep1_pos	Fruit_flour	Individual_12
SA405998	Individual12-rep2_neg_TOP5	Fruit_flour	Individual_12
SA405999	Individual12-rep3_neg	Fruit_flour	Individual_12
SA406000	Individual13-rep1_pos_TOP5	Fruit_flour	Individual_13
SA406001	Individual13-rep2_neg	Fruit_flour	Individual_13
SA406002	Individual13-rep1_pos	Fruit_flour	Individual_13
SA406003	Individual13-rep1_neg_TOP5	Fruit_flour	Individual_13
SA406004	Individual13-rep2_pos	Fruit_flour	Individual_13
SA406005	Individual13-rep1_neg	Fruit_flour	Individual_13
SA406006	Individual13-rep3_pos_TOP5	Fruit_flour	Individual_13
SA406007	Individual13-rep3_neg_TOP5	Fruit_flour	Individual_13
SA406008	Individual13-rep3_pos	Fruit_flour	Individual_13
SA406009	Individual13-rep3_neg	Fruit_flour	Individual_13
SA406010	Individual13-rep2_neg_TOP5	Fruit_flour	Individual_13
SA406011	Individual13-rep2_pos_TOP5	Fruit_flour	Individual_13
SA406012	Individual14-rep1_pos	Fruit_flour	Individual_14
SA406013	Individual14-rep1_pos_TOP5	Fruit_flour	Individual_14
SA406014	Individual14-rep2_pos	Fruit_flour	Individual_14
SA406015	Individual14-rep2_pos_TOP5	Fruit_flour	Individual_14
SA406016	Individual14-rep3_pos	Fruit_flour	Individual_14
SA406017	Individual14-rep3_pos_TOP5	Fruit_flour	Individual_14
SA406018	Individual14-rep3_neg_TOP5	Fruit_flour	Individual_14
SA406019	Individual14-rep3_neg	Fruit_flour	Individual_14
SA406020	Individual14-rep2_neg_TOP5	Fruit_flour	Individual_14
SA406021	Individual14-rep2_neg	Fruit_flour	Individual_14
SA406022	Individual14-rep1_neg_TOP5	Fruit_flour	Individual_14
SA406023	Individual14-rep1_neg	Fruit_flour	Individual_14
SA406024	Individual2-rep1_pos	Fruit_flour	Individual_2
SA406025	Individual2-rep1_pos_TOP5	Fruit_flour	Individual_2
SA406026	Individual2-rep3_neg_TOP5	Fruit_flour	Individual_2
SA406027	Individual2-rep3_pos_TOP5	Fruit_flour	Individual_2
SA406028	Individual2-rep3_neg	Fruit_flour	Individual_2
SA406029	Individual2-rep2_neg_TOP5	Fruit_flour	Individual_2
SA406030	Individual2-rep2_neg	Fruit_flour	Individual_2
SA406031	Individual2-rep1_neg	Fruit_flour	Individual_2
SA406032	Individual2-rep3_pos	Fruit_flour	Individual_2
SA406033	Individual2-rep2_pos_TOP5	Fruit_flour	Individual_2
SA406034	Individual2-rep2_pos	Fruit_flour	Individual_2
SA406035	Individual2-rep1_neg_TOP5	Fruit_flour	Individual_2
SA406036	Individual3-rep1_pos_TOP5	Fruit_flour	Individual_3
SA406037	Individual3-rep1_pos	Fruit_flour	Individual_3
SA406038	Individual3-rep3_neg	Fruit_flour	Individual_3
SA406039	Individual3-rep2_neg_TOP5	Fruit_flour	Individual_3
SA406040	Individual3-rep2_neg	Fruit_flour	Individual_3
SA406041	Individual3-rep1_neg_TOP5	Fruit_flour	Individual_3
SA406042	Individual3-rep1_neg	Fruit_flour	Individual_3
SA406043	Individual3-rep2_pos	Fruit_flour	Individual_3
SA406044	Individual3-rep3_neg_TOP5	Fruit_flour	Individual_3
SA406045	Individual3-rep2_pos_TOP5	Fruit_flour	Individual_3
SA406046	Individual3-rep3_pos	Fruit_flour	Individual_3
SA406047	Individual3-rep3_pos_TOP5	Fruit_flour	Individual_3
SA406048	Individual4-rep3_pos	Fruit_flour	Individual_4
SA406049	Individual4-rep1_pos	Fruit_flour	Individual_4
SA406050	Individual4-rep3_neg_TOP5	Fruit_flour	Individual_4
SA406051	Individual4-rep3_pos_TOP5	Fruit_flour	Individual_4

Showing page 1 of 2 Results: 1 2 Next Showing results 1 to 100 of 188

Collection:

Collection ID:	CO003833
Collection Summary:	Acorns from fourteen different individuals of holm oak were harvested at maturity stage during the 2022 – 2023 season (Supplementary Table 1). Undamaged acorns were bleach disinfected, abundantly washed with tap water, and stored in the dark at 4 °C (Bonner, F. T. (1987). Seed biology and technology of Quercus (Vol. 66). US Department of Agriculture, Forest Service, Southern Forest Experiment Station. Simova-Stoilova, L. P., et al (2015). 2-DE proteomics analysis of drought treated seedlings of Quercus ilex supports a root active strategy for metabolic adaptation in response to water shortage. Frontiers in plant science, 6, 627.; López-Hidalgo, C., et al (2021)). Phytochemical composition and variability in Quercus ilex acorn morphotypes as determined by NIRS and MS-based approaches. Food chemistry, 338, 12780) until flour preparation. Acorns were classified into three levels of bitterness (low, medium and high) according to the guidelines provided by the local people who supplied the samples
Sample Type:	Fruit

Treatment:

Treatment ID:	TR003849
Treatment Summary:	No special treatment was employed. Fruits were processed into flour by grinding in liquid nitrogen.

Sample Preparation:

Sampleprep ID:	SP003846
Sampleprep Summary:	Metabolites were extracted from freeze-dried leaf powder. Briefly, a buffer containing 1200 μL of cold ethanol: water (50:50) was added to 30 mg of flour, tissue disruption was driven by maceration with pistil, vortexed (10 s) and sonicated (ultrasonic bath, 40 kHZ for 10 min). After centrifugation (16,000×g, 4°C, 6 min) the supernatant was vacuum dried at 30 °C (Speedvac, Eppendorf Vacuum Concentrator Plus/5301, Eppendorf, Leicestershire, UK).

Sampleprep ID:

SP003846

Sampleprep Summary:

Metabolites were extracted from freeze-dried leaf powder. Briefly, a buffer containing 1200 μL of cold ethanol: water (50:50) was added to 30 mg of flour, tissue disruption was driven by maceration with pistil, vortexed (10 s) and sonicated (ultrasonic bath, 40 kHZ for 10 min). After centrifugation (16,000×g, 4°C, 6 min) the supernatant was vacuum dried at 30 °C (Speedvac, Eppendorf Vacuum Concentrator Plus/5301, Eppendorf, Leicestershire, UK).

Combined analysis:

Analysis ID	AN006083	AN006084
Analysis type	MS	MS
Chromatography type	Reversed phase	Reversed phase
Chromatography system	Waters Acquity	Waters Acquity
Column	Waters ACQUITY UPLC BEH C8 (100 x 2.1mm,1.7um)	Waters ACQUITY UPLC BEH C8 (100 x 2.1mm,1.7um)
MS Type	Other	Other
MS instrument type	Orbitrap	Orbitrap
MS instrument name	Thermo Q Exactive Orbitrap	Thermo Q Exactive Orbitrap
Ion Mode	POSITIVE	NEGATIVE
Units	Peak area	Peak area

Chromatography:

Chromatography ID:	CH004619
Chromatography Summary:	Chromatographic separation was carried out using an Acquity UPLC BEH C18 column (2.1 x 100 mm, 1.7 µm) (Waters, Manchester, U.K.) maintaining it at 40 °C. The injection volume was 5 µl and the flow rate was set at 0.5 mL/min. Mobile phases consisted of 0.1% formic acid in water (Eluent A) and 0.1% formic acid in methanol (Eluen B). Elution conditions were as follows: 5% B for 1 min, linear gradient from 5% to 100% in solvent B for 9 min, isocratic at 100% B for 2 min, and return to initial conditions, 5% B for 3 min.
Instrument Name:	Waters Acquity
Column Name:	Waters ACQUITY UPLC BEH C8 (100 x 2.1mm,1.7um)
Column Temperature:	40
Flow Gradient:	5% B for 1 min, linear gradient from 5% to 100% in solvent B for 9 min, isocratic at 100% B for 2 min, and return to initial conditions, 5% B for 3 min.
Flow Rate:	0.5 mL/min
Solvent A:	100% water; 0.1% formic acid
Solvent B:	100% methanol; 0.1% formic acid
Chromatography Type:	Reversed phase

MS:

MS ID:	MS005790
Analysis ID:	AN006083
Instrument Name:	Thermo Q Exactive Orbitrap
Instrument Type:	Orbitrap
MS Type:	Other
MS Comments:	MS detection was performed with the Q Exactive Orbitrap mass spectrometer operating in positive and negative polarities. HESI source parameters in positive mode were spray voltage, 3.5 kV; S-lens RF level, 50; capillary temperature, 320 °C; sheath and auxiliary gas flow, 60 and 25, respectively (arbitrary units); and probe heater temperature, 400 ºC. For negative ion mode, all parameters remained the same except that the spray voltage was set to -3.0 kV. Xcalibur v.4.3 software was used for instrument control and data acquisition. A Full Scan MS method was acquired at a resolution of 70,000 (full width half maximum, FWHM at m/z 200) and a data dependent acquisition MS2 method was acquired at resolution 70,000 and 17,500 (FWHM at m/z 200) for Full Scan and Product Ion Scan, respectively, fragmenting the five most abundant precursor ions per MS scan (Top5). Full Scan MS and data dependent acquisition MS2 methods were acquired in positive and negative modes, and mass range used for both experiments was 70 – 1,050 m/z. Additionally, for continuous quality assurance and to promote conﬁdence in the data, quality control (QC) mix was prepared using equal volumes of all samples and was injected after every six samples during the batch processing along with methanol as a blank run to correct for a drift of the raw signal intensity during the analysis. Moreover, the QC samples were analysed in a data-dependent (dd-MS2/dd-SIM) manner for feature annotation. All acquired data were exported by Xcalibur software to be analysed by the Compound Discoverer v3.2 software (Thermo Fisher Scientific, Bremen, Germany)
Ion Mode:	POSITIVE

MS ID:	MS005791
Analysis ID:	AN006084
Instrument Name:	Thermo Q Exactive Orbitrap
Instrument Type:	Orbitrap
MS Type:	Other
MS Comments:	S detection was performed with the Q Exactive Orbitrap mass spectrometer operating in positive and negative polarities. HESI source parameters in positive mode were spray voltage, 3.5 kV; S-lens RF level, 50; capillary temperature, 320 °C; sheath and auxiliary gas flow, 60 and 25, respectively (arbitrary units); and probe heater temperature, 400 ºC. For negative ion mode, all parameters remained the same except that the spray voltage was set to -3.0 kV. Xcalibur v.4.3 software was used for instrument control and data acquisition. A Full Scan MS method was acquired at a resolution of 70,000 (full width half maximum, FWHM at m/z 200) and a data dependent acquisition MS2 method was acquired at resolution 70,000 and 17,500 (FWHM at m/z 200) for Full Scan and Product Ion Scan, respectively, fragmenting the five most abundant precursor ions per MS scan (Top5). Full Scan MS and data dependent acquisition MS2 methods were acquired in positive and negative modes, and mass range used for both experiments was 70 – 1,050 m/z. Additionally, for continuous quality assurance and to promote conﬁdence in the data, quality control (QC) mix was prepared using equal volumes of all samples and was injected after every six samples during the batch processing along with methanol as a blank run to correct for a drift of the raw signal intensity during the analysis. Moreover, the QC samples were analysed in a data-dependent (dd-MS2/dd-SIM) manner for feature annotation. All acquired data were exported by Xcalibur software to be analysed by the Compound Discoverer v3.2 software (Thermo Fisher Scientific, Bremen, Germany)
Ion Mode:	NEGATIVE