Optimizing accelerated solvent extraction combined with liquid chromatography-Orbitrap mass spectrometry for efficient lipid profile characterization of mozzarella cheese

Mentana, Annalisa; Zianni, Rosalia; Campaniello, Maria; Tomaiuolo, Michele; Chiappinelli, Andrea; Iammarino, Marco; Nardelli, Valeria

doi:10.1016/j.foodchem.2022.133542

Cited by 8 publications

(6 citation statements)

References 35 publications

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“…The simultaneous optimization of HS-SPME parameters, conducted with a dedicated CCD, permitted an efficient number of experiments to estimate the effect and interactions of variables [28]. DOM, commonly used in optimization of design parameters [29], was employed to obtain a good compromise among predicted response models obtained from CCD.…”

Section: Optimization Of Hs-spme Extraction By Central Composite Desi...mentioning

confidence: 99%

Headspace Solid-Phase Microextraction/Gas Chromatography–Mass Spectrometry and Chemometric Approach for the Study of Volatile Profile in X-ray Irradiated Surface-Ripened Cheeses

Palermo,

Mentana,

Tomaiuolo

et al. 2024

Foods

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X-ray irradiation is an emerging non-thermal technology that is used as a preservation and sanitization technique to inactivate pathogens and spoilage organisms, increasing the shelf life of products. In this work, two different types of surface-ripened cheeses, Brie and Camembert, produced with cow milk, were treated with X-rays at three dose levels, 2.0, 4.0 and 6.0 kGy, to evaluate the irradiation effects on the volatile profile using a volatolomic approach. The headspace solid-phase microextraction (HS-SPME) technique combined with gas chromatography–mass spectrometry (GC–MS) was used to extract and analyze the volatile fraction from these dairy matrices. The HS-SPME method was optimized by a central composite design in combination with a desirability optimization methodology. The Carboxen/PDMS fiber, 50 °C for extraction temperature and 60 min for time extraction were found to be the best parameter settings and were applied for this investigation. The obtained fingerprints demonstrated that the irradiation-induced changes are dose dependent. The X-ray irradiation produced many new volatiles not found in the non-irradiated samples, but it also varied the amount of some volatiles already present in the control. Specifically, aldehydes and hydrocarbons increased with the irradiation dose, whereas alcohols, carboxylic acids, esters, methyl esters, ketones, lactones and sulfur-containing compounds showed a non-linear dependence on the dose levels; indeed, they increased up to 4.0 kGy, and then decreased slightly at 6.0 kGy. This trend, more evident in the Camembert profile, is probably due to the fact that these compounds are involved in different oxidation mechanisms of lipids and proteins, which were induced by the radiation treatment. In these oxidative chemical changes, the production and degradation processes of the volatiles are competitive, but at higher doses, the decomposition reactions exceed those of formation. A principal component analysis and partial least square discriminant analysis were used to discriminate between the treated and untreated samples. Moreover, this study allowed for the identification of potential markers of X-ray treatment for the two cheeses, confirming this approach as a useful tool for the control of irradiated surface-ripened cheeses.

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Section: Optimization Of Hs-spme Extraction By Central Composite Desi...mentioning

confidence: 99%

Headspace Solid-Phase Microextraction/Gas Chromatography–Mass Spectrometry and Chemometric Approach for the Study of Volatile Profile in X-ray Irradiated Surface-Ripened Cheeses

Palermo,

Mentana,

Tomaiuolo

et al. 2024

Foods

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“…Folch method was carried out on 0.5 g of homogenized mozzarella cheese spiked with 200 µL of working standard solution of trinonanoin as internal standard. The extraction procedure was performed according to our previous article [11].…”

Section: Folch Proceduresmentioning

confidence: 99%

“…During the search, the software compared each "data-dependent" mass spectrum with the proprietary library containing thousands of lipids mass spectra. Each peak was classified with a score resulting from overlap with the theoretical spectra, providing a highly accurate identification of the fatty acid composition and sn1, sn2, or sn3 position [11]. Detailed software parameters are reported in Table S1.…”

Section: Untargeted Analysismentioning

confidence: 99%

“…Matyash et al [9] introduced methyl-tert-butyl ether (MTBE) as a non-toxic solvent for the extraction of lipids from biological samples; this solvent was also associated with other techniques, such as ultrasound extraction [10]. Recently, Accelerated Solvent Extraction (ASE) was proposed as an alternative and efficient solvent extraction technique for lipid analysis [11]; this automated technique, through the use of high temperature and pressure, allows for reducing the quantity of organic solvent necessary for extraction and the process times [12].…”

Section: Introductionmentioning

confidence: 99%

“…In our previous research, untargeted lipid fingerprints of soft cheeses were studied by successfully applying Folch and ASE extraction techniques [11] and evaluating the effect of technological processes on the lipid composition of cheese [3]. However, to our knowledge, no studies using MAE associated with untargeted lipidomics have been reported.…”

Section: Introductionmentioning

confidence: 99%

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Microwave-Assisted Extraction/UHPLC-Q-Orbitrap-MS-Based Lipidomic Workflow for Comprehensive Study of Lipids in Soft Cheese

Campaniello,

Nardelli,

Zianni

et al. 2024

Foods

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In this work, Microwave-Assisted Extraction (MAE) was proposed as an alternative and environmentally friendly technique in lipidomics to study the lipid fingerprint of soft cheeses, such as mozzarella. For method development, a first step concerning an evaluation of extraction solvents was carried out via testing three different mixtures, including methanol/ethyl acetate, isopropanol/ethyl acetate, and ethanol/ethyl acetate, at a 1:2 v/v ratio. The latter was chosen as a solvent mixture for subsequent method optimization. MAE conditions, in terms of solvent volume, time, and temperature, were explored to define their effects on extraction capability through a full factorial experimental design. The best compromise to extract more lipids at the same time was obtained with 24 mL g−1 for solvent-to-solid ratio, 65 °C for temperature, and 18 min for time. Lipid analyses were conducted by UHPLC-Q-Orbitrap-MS associated with multivariate statistics. The developed lipidomic workflow allowed for the extraction of over 400 lipids grouped into 18 different subclasses. The results confirmed that MAE is a suitable technique for lipid extraction in the omics approach with high efficiency, even using low-cost and less toxic solvents. Moreover, a comprehensive structure characterization of extracted lipids, in terms of fatty acid composition and regiochemistry, was carried out.

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Sampling and sample preparation methods for the determination of the volatile components of milk and dairy products

Chen,

Zheng,

Costa

2024

Reference Module in Chemistry, Molecular Sciences and Chemical Engineering

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Optimizing accelerated solvent extraction combined with liquid chromatography-Orbitrap mass spectrometry for efficient lipid profile characterization of mozzarella cheese

Cited by 8 publications

References 35 publications

Headspace Solid-Phase Microextraction/Gas Chromatography–Mass Spectrometry and Chemometric Approach for the Study of Volatile Profile in X-ray Irradiated Surface-Ripened Cheeses

Headspace Solid-Phase Microextraction/Gas Chromatography–Mass Spectrometry and Chemometric Approach for the Study of Volatile Profile in X-ray Irradiated Surface-Ripened Cheeses

Microwave-Assisted Extraction/UHPLC-Q-Orbitrap-MS-Based Lipidomic Workflow for Comprehensive Study of Lipids in Soft Cheese

Sampling and sample preparation methods for the determination of the volatile components of milk and dairy products

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