Analytical Platforms for the Determination of Phospholipid Turnover in Breast Cancer Tissue: Role of Phospholipase Activity in Breast Cancer Development.

Altered lipid metabolism has been associated with the progression of various cancers, and aberrant expression of enzymes involved in the lipid metabolism has been detected in different stages of cancer. Breast cancer (BC) is one of the cancer types known to be associated with alterations in the lipid metabolism and overexpression of enzymes involved in this metabolism. It has been demonstrated that inhibition of the activity of certain enzymes, such as that of phospholipase A in BC cell lines sensitizes these cells and decreases the IC values for forthcoming therapy with traditional drugs, such as doxorubicin and tamoxifen.

Monitoring Phthalates in Table and Fortified Wines by Headspace Solid-Phase Microextraction Combined with Gas Chromatography-Mass Spectrometry Analysis.

Phthalates are a class of endocrine disruptors extensively used in plastic production as plasticizers, and as a result, they can be found in foods as a result of their migration ability. The occurrence of phthalates was monitored in 20 Portuguese wines using a simple, reliable, and environmentally friendly analytical method, headspace solid-phase microextraction combined with gas chromatography-mass spectrometry. Satisfactory figures of merit of method, linearity (correlation coefficient of ≥0.

Lipid biosignature of breast cancer tissues by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.

Purpose: One of the hallmarks of cancer cells is the demand of supply for the synthesis of new membranes involved in cell proliferation and lipids have an important role in cellular structure, signaling pathways and progression of cancer. In this sense, lipid studies have become an essential tool allowing the establishment of signatures associated with breast cancer (BC). In this regard, some metabolic processes including proteins, nucleic acids and lipid synthesis are enhanced as part of cancer-associated metabolic reprogramming, as a requirement for cell growth and proliferation.

Untargeted Urinary H NMR-Based Metabolomic Pattern as a Potential Platform in Breast Cancer Detection.

Breast cancer (BC) remains the second leading cause of death among women worldwide. An emerging approach based on the identification of endogenous metabolites (EMs) and the establishment of the metabolomic fingerprint of biological fluids constitutes a new frontier in medical diagnostics and a promising strategy to differentiate cancer patients from healthy individuals. In this work we aimed to establish the urinary metabolomic patterns from 40 BC patients and 38 healthy controls (CTL) using proton nuclear magnetic resonance spectroscopy (1H-NMR) as a powerful approach to identify a set of BC-specific metabolites which might be employed in the diagnosis of BC.

Comparison of high-throughput microextraction techniques, MEPS and μ-SPEed, for the determination of polyphenols in baby food by ultrahigh pressure liquid chromatography.

In this study, two different high-throughput microextraction techniques, microextraction by packed sorbents (MEPS) and micro solid phase extraction (μ-SPEed®), were evaluated and compared, regarding the performance criteria, for the isolation of polyphenols from baby foods prior to their determination by ultrahigh pressure liquid chromatography (UHPLC). To achieve the best performance, influential parameters affecting extraction efficiency (including type of sorbent, number of extraction cycles, pH, elution solvent and elution volume) were systematically studied and optimized. To enable an effective comparison, selectivity, linear dynamic range, method detection (LODs) and quantification limits (LOQs), accuracy, precision and extraction yields, were determined and discussed for both techniques.

Implementing a central composite design for the optimization of solid phase microextraction to establish the urinary volatomic expression: a first approach for breast cancer.

Introduction: Breast cancer (BC) is positioned as the second among all cancers remaining at the top of women´s diseases worldwide followed by colorectum, lung, cervix, and thyroid cancers. The main drawback of most the screening/diagnostic methods is their low sensitivity/specificity and in some cases the invasive procedure required to obtain the samples.

Objectives: On the present investigation, we report a statistical design was to evaluate by central composite design the influence towards the optimization of the most significant variables of solid-phase microextraction (SPME) procedure for the isolation of volatile organic metabolites (VOMs) from urine of BC patients (N = 31) and healthy individuals (CTL; N = 40).

Impact of storage time and temperature on volatomic signature of Tinta Negra wines by LLME/GC-MS.

The current study reports the effect of storage temperature, storage time and glucose content on the volatomic signature of Tinta Negra wines using liquid-liquid microextraction (LLME) combined with gas chromatography-ion trap mass spectrometry (GC-MS). A total of 65 volatile organic compounds (VOCs) were identified in Tinta Negra, of which only 14 appear during storage. Based on the results, the freshness and fruitiness odours that are related to the presence of some varietal and fermentative components (e.

Establishment of the Volatile Signature of Wine-Based Aromatic Vinegars Subjected to Maceration.

The flavoring of vinegars with aromatic fruits and medicinal herbs is a practice with increasing trend mostly in countries with oenological tradition, resulting in a product of improved quality and consumer attractiveness. This study was directed towards the evaluation of the impact of the maceration process on the volatile signature of wine-based aromatic vinegars (WBAVs). The evaluation was performed using solid phase microextraction (SPME) combined with gas chromatography combined with mass spectrometry (GC-MS).

A useful strategy based on chromatographic data combined with quality-by-design approach for food analysis applications. The case study of furanic derivatives in sugarcane honey.

Sugarcane honey (SCH) is one of the Madeira Island products par excellence and it is now popular worldwide. Its sui generis and peculiar sensory properties, explained by a variety of volatile compounds including furanic derivatives (FDs), arise mainly from manufacturing and storage conditions. A simple high-throughput approach based on semi-automatic microextraction by packed sorbent (MEPS) combined with ultra-high performance liquid chromatography (UHPLC) was developed and validated for identification and quantification of target FDs in sugarcane honey.

Volatile metabolomic signature of human breast cancer cell lines.

Breast cancer (BC) remains the most prevalent oncologic pathology in women, causing huge psychological, economic and social impacts on our society. Currently, the available diagnostic tools have limited sensitivity and specificity. Metabolome analysis has emerged as a powerful tool for obtaining information about the biological processes that occur in organisms, and is a useful platform for discovering new biomarkers or make disease diagnosis using different biofluids.

A powerful approach to explore the potential of medicinal plants as a natural source of odor and antioxidant compounds.

In this study an efficient and reliable method based on dynamic headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-qMS), was developed to establish the volatile metabolomic pattern of Thymus vulgaris L., Rosmarinus officinalis L. and Ruta chalepensis L.

Determination of urinary levels of leukotriene B(4) using ad highly specific and sensitive methodology based on automatic MEPS combined with UHPLC-PDA analysis.

Leukotriene B4 (LTB4) is a potent mediator of inflammation and plays a key function in the pathophysiology of chronic asthma. Detectable urinary levels of LTB4, arises from the activation of leukotriene pathways. In this study an ultra-fast, selective and sensitive analytical method based on semi-automatic microextraction by packed sorbents (MEPS) technique, using a new digitally controlled syringe (eVol®) combined with ultra-high pressure liquid chromatography (UHPLC), is proposed for the measurement of urinary LTB4 (U-LTB4) levels in a group of asthmatic patients (APs) and healthy controls (CTRL).

Quantification of furanic derivatives in fortified wines by a highly sensitive and ultrafast analytical strategy based on digitally controlled microextraction by packed sorbent combined with ultrahigh pressure liquid chromatography.

An improved, reliable and powerful analytical strategy based on digitally controlled microextraction by packed sorbent (MEPS) combined with ultrahigh pressure liquid chromatography (UHPLC) was validated for the simultaneous identification and quantification of major furanic derivatives, namely 5-hydroxymethyl-2-furaldehyde (5HMF), 5-methyl-2-furaldehyde (5MF), 2-furaldehyde (2F) and 2-furyl methyl ketone (2FMK), in fortified wines. To enhance the extraction efficiency of the target furanic derivates, several influencing extraction parameters, such as number of loading cycles, nature of elution solvent and elution volume, were evaluated and optimized. In addition the ability of different MEPS sorbent materials, namely C2, C8, C18, SIL, M1, R-AX, R-CX and PGC, were also tested.

A powerful methodological approach combining headspace solid phase microextraction, mass spectrometry and multivariate analysis for profiling the volatile metabolomic pattern of beer starting raw materials.

The volatile metabolomic patterns from different raw materials commonly used in beer production, namely barley, corn and hop-derived products - such as hop pellets, hop essential oil from Saaz variety and tetra-hydro isomerized hop extract (tetra hop), were established using a suitable analytical procedure based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography-quadrupole mass spectrometry detection (GC-qMS). Some SPME extraction parameters were optimized. The best results, in terms of maximum signal recorded and number of isolated metabolites, were obtained with a 50/30 μm DVB/CAR/PDMS coating fiber at 40 °C for 30 min.

Re-exploring the high-throughput potential of microextraction techniques, SPME and MEPS, as powerful strategies for medical diagnostic purposes. Innovative approaches, recent applications and future trends.

The human population continues to grow exponentially in the fast developing and most populated countries, whereas in Western Europe it is getting older and older each year. This inevitably raises the demand for better and more efficient medical services without increasing the economic burden in the same proportion. To meet these requirements, improvement of medical diagnosis is certainly a key aspect to consider.

A new and improved strategy combining a dispersive-solid phase extraction-based multiclass method with ultra high pressure liquid chromatography for analysis of low molecular weight polyphenols in vegetables.

This paper reports on the development and optimization of a modified Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) based extraction technique coupled with a clean-up dispersive-solid phase extraction (dSPE) as a new, reliable and powerful strategy to enhance the extraction efficiency of free low molecular-weight polyphenols in selected species of dietary vegetables. The process involves two simple steps. First, the homogenized samples are extracted and partitioned using an organic solvent and salt solution.

A sensitive microextraction by packed sorbent-based methodology combined with ultra-high pressure liquid chromatography as a powerful technique for analysis of biologically active flavonols in wines.

A new approach based on microextraction by packed sorbent (MEPS) and reversed-phase high-throughput ultra high pressure liquid chromatography (UHPLC) method that uses a gradient elution and diode array detection to quantitate three biologically active flavonols in wines, myricetin, quercetin, and kaempferol, is described. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (selectivity, linearity, sensitivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters such as the type of sorbent material (C2, C8, C18, SIL, and C8/SCX), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, on the MEPS performance. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250μL) in five extraction cycle and in a short time period (about 5min for the entire sample preparation step).

Development of a novel microextraction by packed sorbent-based approach followed by ultrahigh pressure liquid chromatography as a powerful technique for quantification phenolic constituents of biological interest in wines.

A novel analytical approach, based on a miniaturized extraction technique, the microextraction by packed sorbent (MEPS), followed by ultrahigh pressure liquid chromatography (UHPLC) separation combined with a photodiode array (PDA) detection, has been developed and validated for the quantitative determination of sixteen biologically active phenolic constituents of wine. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (linearity, sensitivity, selectivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters on the MEPS performance such as the type of sorbent material (C2, C8, C18, SIL, and M1), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, were studied. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250 μL) in five extraction cycle and in a short time period (about 5 min for the entire sample preparation step).

Solid phase microextraction, mass spectrometry and metabolomic approaches for detection of potential urinary cancer biomarkers--a powerful strategy for breast cancer diagnosis.

A sensitive assay to identify volatile organic metabolites (VOMs) as biomarkers that can accurately diagnose the onset of breast cancer using non-invasively collected clinical specimens is ideal for early detection. Therefore the aim of this study was to establish the urinary metabolomic profile of breast cancer patients and healthy individuals (control group) and to explore the VOMs as potential biomarkers in breast cancer diagnosis at early stage. Solid-phase microextraction (SPME) using CAR/PDMS sorbent combined with gas chromatography-mass spectrometry was applied to obtain metabolomic information patterns of 26 breast cancer patients and 21 healthy individuals (controls).

A fast method using a new hydrophilic-lipophilic balanced sorbent in combination with ultra-high performance liquid chromatography for quantification of significant bioactive metabolites in wines.

This manuscript describes the development and validation of an ultra-fast, efficient, and high throughput analytical method based on ultra-high performance liquid chromatography (UHPLC) equipped with a photodiode array (PDA) detection system, for the simultaneous analysis of fifteen bioactive metabolites: gallic acid, protocatechuic acid, (-)-catechin, gentisic acid, (-)-epicatechin, syringic acid, p-coumaric acid, ferulic acid, m-coumaric acid, rutin, trans-resveratrol, myricetin, quercetin, cinnamic acid and kaempferol, in wines. A 50-mm column packed with 1.7-μm particles operating at elevated pressure (UHPLC strategy) was selected to attain ultra-fast analysis and highly efficient separations.