Summary of Study ST002570
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 PR001657. The data can be accessed directly via it's Project DOI: 10.21228/M8HQ62 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.
| Study ID | ST002570 |
| Study Title | Evaluation of Extraction Parameters for the Analysis of Lipid Classes in Plants |
| Study Summary | The aim of this study was to preliminary evaluate the lipid profile alterations on Pitcairnia flammea leaves based on variations in solvent proportion and ultrasonic ice bath extraction time, followed by a lipid class-enriched analysis employing chemometric techniques. In the plant extraction method employed, the sample was separated in 3 phases 2 : organic, aqueous and protein phases. The parameters evaluated in our study were different solvent proportion (1:2, 1:3 or 1:4 v/v) and time under ultrasonic in ice-cold bath (10, 20 or 30 min). The extraction solvents were methanol (MeOH) and methyl tert-butyl ether (MTBE). For each condition, experiments were prepared in triplicate resulting in 27 samples. Samples extracted in MeOH:MTBE (1:2 v/v) for 10 min and 20 min ultrasonic bath did not separate in three phases. Then, their organic phase chromatographic analyses were not performed resulting on 42 experimental samples chromatograms. Ultra-high performance liquid chromatography coupled to electrospray ionization mass spectrometry (UHPLC-ESI-MS) was used to acquire raw data and MS-DIAL and MetaboAnalyst platforms were used to perform data preprocessing and statistical analysis. The statistical analysis of UHPLC-ESI-MS data in both ionization modes enabled the visualization of a trend distribution based on extraction time. Furthermore, we were able to establish that the solvent proportion had a greater impact on group separation in data samples extracted for 30 min versus 10 and 20 min. Moreover, diacylglycerol or/and lysophophatidylcholine are lipid subclasses that can be favored depending on the extraction time in the MS analyses using positive ESI mode. |
| Institute | University of Campinas |
| Department | Chemistry's Institute |
| Laboratory | Laboratory of Bioanalytics and Integrated Omics |
| Last Name | Matos |
| First Name | Taynara |
| Address | Rua Josué de Castro, s/n – Cidade Universitária, 13083-970, Campinas – SP, Brazil |
| t262827@dac.unicamp.br | |
| Phone | (85)996154192 |
| Submit Date | 2023-04-17 |
| Raw Data Available | Yes |
| Raw Data File Type(s) | raw(Thermo) |
| Analysis Type Detail | LC-MS |
| Release Date | 2023-06-01 |
| Release Version | 1 |
Select appropriate tab below to view additional metadata details:
Project:
| Project ID: | PR001657 |
| Project DOI: | doi: 10.21228/M8HQ62 |
| Project Title: | Plant lipidomics studies |
| Project Type: | MS untargeted analysis |
| Project Summary: | Untargeted analysis on Bromeliades leaf samples. The aim of this study was to preliminary evaluate the lipid profile alterations on Pitcairnia flammea leaves based on variations in solvent proportion and ultrasonic ice bath extraction time, followed by a lipid class-enriched analysis employing chemometric techniques. |
| Institute: | University of Campinas |
| Department: | Chemistry's Institute |
| Laboratory: | Laboratory of Bioanalytics and Integrated Omics |
| Last Name: | Matos |
| First Name: | Taynara |
| Address: | Rua Josué de Castro, s/n – Cidade Universitária, 13083-970, Campinas – SP, Brazil |
| Email: | t262827@dac.unicamp.br |
| Phone: | (85)996154192 |
Subject:
| Subject ID: | SU002671 |
| Subject Type: | Plant |
| Subject Species: | Pitcairnia flammea |
| Species Group: | Plants |
Factors:
Subject type: Plant; Subject species: Pitcairnia flammea (Factor headings shown in green)
| mb_sample_id | local_sample_id | Time | Solvent | Sample_type |
|---|---|---|---|---|
| SA258294 | A2_2-NEG | 10 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258295 | A2_3-NEG | 10 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258296 | A2_1-POS | 10 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258297 | A2_1-NEG | 10 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258298 | A2_2-POS | 10 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258299 | A2_3-POS | 10 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258300 | A3_1-POS | 10 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258301 | A3_3-POS | 10 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258302 | A3_2-NEG | 10 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258303 | A3_3-NEG | 10 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258304 | A3_2-POS | 10 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258305 | A3_1-NEG | 10 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258306 | B2_3-POS | 20 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258307 | B2_2-NEG | 20 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258308 | B2_3-NEG | 20 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258309 | B2_1-POS | 20 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258310 | B2_2-POS | 20 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258311 | B2_1-NEG | 20 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258312 | B3_2-POS | 20 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258313 | B3_1-POS | 20 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258314 | B3_2-NEG | 20 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258315 | B3_3-NEG | 20 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258316 | B3_3-POS | 20 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258317 | B3_1-NEG | 20 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258318 | C1_2-NEG | 30 min | MeOH;MTBE (1;2 v/v) | Sample |
| SA258319 | C1_3-NEG | 30 min | MeOH;MTBE (1;2 v/v) | Sample |
| SA258320 | C1_3-POS | 30 min | MeOH;MTBE (1;2 v/v) | Sample |
| SA258321 | C1_2-POS | 30 min | MeOH;MTBE (1;2 v/v) | Sample |
| SA258322 | C1_1-NEG | 30 min | MeOH;MTBE (1;2 v/v) | Sample |
| SA258323 | C1_1-POS | 30 min | MeOH;MTBE (1;2 v/v) | Sample |
| SA258324 | C2_2-NEG | 30 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258325 | C2_3-NEG | 30 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258326 | C2_1-POS | 30 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258327 | C2_1-NEG | 30 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258328 | C2_2-POS | 30 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258329 | C2_3-POS | 30 min | MeOH;MTBE (1;3 v/v) | Sample |
| SA258330 | C3_1-NEG | 30 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258331 | C3_1-POS | 30 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258332 | C3_2-NEG | 30 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258333 | C3_3-NEG | 30 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258334 | C3_3-POS | 30 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258335 | C3_2-POS | 30 min | MeOH;MTBE (1;4 v/v) | Sample |
| SA258336 | QC4-NEG | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258337 | QC5-NEG | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258338 | QC7-POS | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258339 | QC7-NEG | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258340 | QC6-NEG | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258341 | QC02-NEG | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258342 | QC02-POS | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258343 | QC01-POS | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258344 | QC6-POS | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258345 | QC5-POS | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258346 | QC4-POS | Pooled QC | Pooled QC | Quality Control (QC) |
| SA258347 | QC01-NEG | Pooled QC | Pooled QC | Quality Control (QC) |
| Showing results 1 to 54 of 54 |
Collection:
| Collection ID: | CO002664 |
| Collection Summary: | Leaves of cultivated Pitcairnia flammea were harvested, and immediately frozen in liquid nitrogen, followed the -80ºC storage until sample preparation. |
| Sample Type: | Leaves |
| Collection Location: | Institute of Biology (UNICAMP, Brazil) |
Treatment:
| Treatment ID: | TR002683 |
| Treatment Summary: | Leaves were macerated to fine powder using a mortar and pestle in liquid nitrogen condition. |
Sample Preparation:
| Sampleprep ID: | SP002677 |
| Sampleprep Summary: | Lipid extraction was based on Hummel et al. Method. 10 mL of solvent mixture were prepared in 3 different proportions - 1:2, 1:3 or 1:4 (v/v) -, pre-cooled at 20 ºC methanol (MeOH) and methyl tert-butyl ether (MTBE). In 2 mL tubes, 50 mg of macerated sample were added and 1 mL of the solvent mixture. The samples were incubated for 5 min under agitation at 500 rpm at 4 ºC, followed by an ultrasonication in ice-cold bath in different times (10, 20, 30 minutes). Each condition was performed in technical triplicate, totalizing 27 samples. After adding 500 µL mixture of water type I:MeOH (3:1 v/v), the samples were vortexed and centrifuged for 5 min at 4 ºC, 10000 rpm. The three phases were separated and dried in a vacuum concentrator, at ambient temperature under vacuum - alcoholic mode, and stored at -80 ºC until the chromatographic analysis. |
Combined analysis:
| Analysis ID | AN004234 | AN004235 |
|---|---|---|
| Analysis type | MS | MS |
| Chromatography type | Reversed phase | Reversed phase |
| Chromatography system | Thermo Scientific UltiMate™ 3000 UHPLC RSLCnano system | Thermo Scientific UltiMate™ 3000 UHPLC RSLCnano system |
| Column | Supelco Sigma-Aldrich Titan C18 column (100 mm x 2.1 mm x 1.9 µm) | Supelco Sigma-Aldrich Titan C18 column (100 mm x 2.1 mm x 1.9 µm) |
| MS Type | ESI | ESI |
| MS instrument type | Orbitrap | Orbitrap |
| MS instrument name | Thermo Q Exactive Orbitrap | Thermo Q Exactive Orbitrap |
| Ion Mode | NEGATIVE | POSITIVE |
| Units | Peak area | Peak area |
Chromatography:
| Chromatography ID: | CH003142 |
| Instrument Name: | Thermo Scientific UltiMate™ 3000 UHPLC RSLCnano system |
| Column Name: | Supelco Sigma-Aldrich Titan C18 column (100 mm x 2.1 mm x 1.9 µm) |
| Column Temperature: | 40 |
| Flow Gradient: | 250 µL/min: 0-2 min: 40% B, 2-3 min: 50% B, 3-6 min: 50% B, 6.1-8 min: 70% B, 8-9 min: 100% B, 9-11 min: 100% B, 11-12 min: 40% B, 12-14 min: 40% B. |
| Flow Rate: | 250 µL/min |
| Solvent A: | 40% acetonitrile/60% water; 10 mM ammonium acetate |
| Solvent B: | 10% acetonitrile/90% isopropanol; 10 mM ammonium acetate |
| Chromatography Type: | Reversed phase |
MS:
| MS ID: | MS003981 |
| Analysis ID: | AN004234 |
| Instrument Name: | Thermo Q Exactive Orbitrap |
| Instrument Type: | Orbitrap |
| MS Type: | ESI |
| MS Comments: | - |
| Ion Mode: | NEGATIVE |
| MS ID: | MS003982 |
| Analysis ID: | AN004235 |
| Instrument Name: | Thermo Q Exactive Orbitrap |
| Instrument Type: | Orbitrap |
| MS Type: | ESI |
| MS Comments: | - |
| Ion Mode: | POSITIVE |
