This study aims to propose a new method for derivatizing fatty acids (FAs) from human milk (HM), eliminating the lipid extraction step, and simplifying the preparation for gas chromatography with a flame ionization detection (GC-FID) analysis to quantify the FAs. The Design Expert software optimized the reaction times, concentrations, and sample amount. The proposed method (PM) was validated for lyophilized HM and results for the figures of merit for precision in relative standard deviation (RSD) (RSDintra-day 1.34-4.03% and RSDinter day 2.08 5.16%), accuracy (99.87-102.16%), and robustness are within a linear range of 3 to 38% lipids in HM samples. The atmospheric solids analysis probe tandem mass spectrometry (ASAP-MS/MS) technique confirmed the efficiency of PM by expressing the molecular composition of triacylglycerol formed by FAs from the GC-FID technique. The PM requires a small sample size and conducts derivatization directly in the sample matrix, minimizing extraction errors. (FAs HM, , (HM) step GCFID GC FID (GC-FID times concentrations amount (PM RSD (RSD RSDintraday RSDintra 1.344.03% 134403 1.34 4.03% 1 34 4 03 1.34-4.03 208 2 08 2.0 5.16%, 516 5.16% 5 16 5.16%) 99.87102.16%, 998710216 99.87 102.16% 99 87 102 (99.87-102.16%) 38 samples ASAPMS/MS ASAPMSMS ASAP MS/MS MS (ASAP-MS/MS matrix errors (HM 344 1.344.03 13440 134 1.3 403 4.03 0 1.34-4.0 20 2. 51 5.16 87102 99.87102.16% 99871021 9987 99.8 10216 102.16 9 8 10 (99.87-102.16% ASAPMS MSMS 1.344.0 1344 13 1. 40 4.0 1.34-4. 5.1 8710 99.87102.16 9987102 998 99. 1021 102.1 (99.87-102.16 1.344. 4. 1.34-4 5. 871 99.87102.1 998710 102. (99.87-102.1 1.344 1.34- 99.87102. 99871 (99.87-102. 99.87102 (99.87-102 99.8710 (99.87-10 99.871 (99.87-1 (99.87- (99.87 (99.8 (99. (99 (9 (

Reuse made by the separation of whey can reduce the waste of human milk. However, the authors are not aware of the literature on treatments in human whey, made available by pasteurization holder, freeze-drying, spray drying, and high hydrostatic pressure. In this context, the present study applied treatments to human whey and evaluated their lipid and immunological quality. Among the results, a different formation in the triacylglycerol profile was evidenced after the application of spray drying and high hydrostatic pressure, while pasteurization and freeze-drying presented ion intensity close to the control human whey. In addition, pasteurization proved to be adequate for lipid nutritional quality and transformation factor-β1 (TGF-β1) concentration, while an increase in interleukin-10 (IL-10) levels was promoted, between 73 and 80%, after freeze-drying, spray drying, and high hydrostatic pressure. Through the principal component analysis, it is noteworthy that the processes presented divergences in terms of the effects caused, with similarity only between pasteurization and freeze-drying in the composition of fatty acids. However, it was observed that all processes were able to maintain the nutrients. Nevertheless, it is relevant to consider individual characteristics presented and the interest in the desired quality, which can be promising as a complementary product to infant feeding. milk However holder freezedrying, freezedrying freeze pressure context results addition factorβ1 factorβ factor β1 β factor-β TGFβ1 TGFβ TGF (TGF-β1 concentration interleukin10 interleukin 10 interleukin-1 IL10 IL (IL-10 promoted 7 80 80% analysis caused acids nutrients Nevertheless feeding (TGF-β interleukin1 1 interleukin- IL1 (IL-1 8 (IL- (IL

The full process of fresh egg preservation presents limitations and is associated with high transportation costs, while processed powdered eggs offer numerous advantages, such as high stability against degradation, providing extended shelf life, easy production, transportation, and favorable storage conditions. Traditional methods for determining the proximate composition of eggs and derivatives lack the capability to eliminate the matrix effect and do not guarantee adequate precision of the results. Therefore, Certified Reference Material (CRM) are the most suitable and effective tool to achieve this purpose. However, in Brazil, CRMs for powdered egg matrix are currently unavailable, although it is not possible to eliminate matrix effects, these can be included in the measurement uncertainty of each CRM. This study aimed to develop a candidate CRM for the powdered egg matrix with the requirements for the competence of testing and calibration laboratories (17034:2016) for proximate composition analyses. The analysis of variance (ANOVA) results for stability and homogeneity indicated no significant variation among the data obtained in the tests and the storage time of the material. Consequently, it was concluded that the powdered egg matrix is stable under simulated transportation conditions (short-term stability) as well as storage conditions (long-term stability) and exhibits adequate homogeneity for a CRM candidate. costs advantages degradation life production Therefore (CRM purpose However Brazil unavailable effects 170342016 17034 2016 (17034:2016 analyses ANOVA (ANOVA material Consequently shortterm short term longterm long 17034201 1703 201 (17034:201 1703420 170 20 (17034:20 170342 17 2 (17034:2 1 (17034: (17034 (1703 (170 (17 (1 (

Olive oil is a highly demanded product renowned for its unique taste and diverse nutrient content, primarily composed of lipids. This study aimed to comprehensively analyze the lipid profiles of four olive varieties (Arbequina, Arbosana, Koroneiki, and Frantoio) and their corresponding commercial olive oils using advanced analytical techniques, namely electrospray ionization mass spectrometry and gas chromatography with flame ionization detector, combined with principal component analysis. The nutritional quality of the olive oils was evaluated based on parameters such as the ratio of saturated acids to polyunsaturated acids, atherogenicity, thrombogenicity, and andhypocholesterolemic/hypercholesterolemic indexes. The study revealed that the primary fatty acids identified were palmitic, stearic, oleic, and linoleic acids, while triolein, palmitodiolein, and stearodiolein emerged as the most abundant triacylglycerol across all samples. Furthermore, the results demonstrated that the commercial olive oil samples exhibited an exceptional nutritional profile. Overall, this study highlights the significance and efficacy of the analytical and statistical techniques employed to unravel the lipid profiles of olive oils, a product of substantial commercial value and susceptible to adulteration. Additionally, it emphasizes the importance of utilizing nutritional quality indices to assess the health benefits associated with olive oil consumption. content lipids Arbequina, Arbequina (Arbequina Arbosana Koroneiki Frantoio detector analysis atherogenicity thrombogenicity andhypocholesterolemichypercholesterolemic andhypocholesterolemic hypercholesterolemic indexes palmitic stearic oleic triolein palmitodiolein Furthermore profile Overall adulteration Additionally consumption

This study describes the validation of a headspace gas chromatography with flame ionization (HS-GC-FID) method for the determination of propanal, pentanal, hexanal, octanal, and trans-2-nonenal originated by lipid oxidation from cat food samples, as well as the evaluation of the matrix effect in the results. This method was applied to the analysis of commercial cat food and proved to be suitable for the determination of these volatile compounds in different samples. Mean recoveries between 88 and 109% were obtained and repeatability expressed as relative standard deviation was always lower than 6.95%. The intra- and inter-assay precisions ranged from 0.44 to 20.88% and from 0.45 to 20.52%, respectively. In addition, the matrix effect of cat food samples was determined by comparing the slopes of the standard addition method, and the external calibration curve and its influences were verified. These results highlight the high potential of this method, which allows the determination of lipid oxidation products in cat food samples directly, without requiring prior sample preparation techniques. HSGCFID HS GC FID (HS-GC-FID propanal pentanal hexanal octanal trans2nonenal transnonenal trans 2 nonenal 8 109 695 6 95 6.95% intra interassay inter assay 044 0 44 0.4 2088 20 20.88 045 45 2052 52 20.52% respectively verified directly techniques 10 69 9 6.95 04 4 0. 208 20.8 205 5 20.52 1 6.9 20. 20.5 6.

The objective of this study was to evaluate the effect of pasteurization, lyophilization and spray-drying on the lipid profile of donated human milk (DHM) at different lactation stages. Nine frozen samples of colostrum, transitional and raw mature human milk (HM) were collected from the Human Milk Bank (HMB) of the Hospital Universitário de Maringá (HUM). Samples were thawed and pooled according to lactation stage. Thereafter, it was submitted to pasteurization, lyophilization and spray-drying processes and later the fatty acid (FA) composition and the lipid profile analyses were performed. Gas chromatograph (GC) with flame ionization detector (FID) and electrospray ionization (ESI) mass spectrometer (MS) were used, respectively. In the FA composition analysis, it was observed that the same classes of saturated FA (SFA), monounsaturated FA (MUFA) and polyunsaturated FA (PUFA) were preserved throughout the process and in all lactation stages. The lipid profiles were also preserved after processing. Therefore, the lyophilization and spray-drying processes are promising techniques to preserve the DHM in the HMB, once the components evaluated were preserved, and both techniques facilitate the transport and storage, as the techniques reduce the sample volume. pasteurization spraydrying spray drying (DHM stages colostrum HM (HM HMB (HMB HUM. HUM . (HUM) stage Thereafter (FA performed GC (GC FID (FID ESI (ESI MS (MS used respectively analysis SFA, SFA , (SFA) MUFA (MUFA PUFA (PUFA processing Therefore storage volume (HUM (SFA

Colostrum human milk samples obtained from human milk banks received different treatments and were evaluated for their proximal composition, fatty acids composition and lipid quality. The total lipids content was maintained in the treatments. There was no difference in moisture, ash, total proteins, carbohydrates and energetic value for raw colostrum human milk and pasteurized colostrum human milk, and there was difference in ash, total proteins and energetic value for freeze-dried colostrum human milk and pasteurized + freeze-dried colostrum human milk. The fatty acids composition demonstrated no difference in the processes for 14 of 31 fatty acids identified. Furthermore, lipid quality indices were obtained, which were unpublished for colostrum human milk submitted to pasteurization and freeze drying. Principal component analysis showed similar behaviors for freeze-dried colostrum human milk and pasteurized and freeze-dried colostrum human milk. So, the processes used may be promising for application in colostrum human milk, due to the maintenance of its proximal characteristics and fatty acid composition. moisture ash freezedried dried 1 3 identified Furthermore drying So

A fast, sensitive, and selective direct injection electrospray tandem mass spectrometry (DI ESI MS/MS) method that is able to quantify ethyl carbamate in commercial sweetened sugar cane spirit is described. The preparation method uses a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) with potassium carbonate added to sweetened sugar cane spirit to separate the aqueous phase from the ethanol phase. The aqueous phase contains sucrose that suppresses electrospray ionization. Ethyl carbamate supernatant from the ethanol phase is transferred and enriched with 18-crown-6/trifluoroacetic acid additives. The additives sequester metal cations reducing the ionization of sodium and potassium, favoring the detection of ethyl carbamate as sole protonated cations. The method was successfully applied for the quantification of eleven real samples and certified sugar cane spirit demonstrating its applicability for quality control and regulatory analysis. The method showed reliable analytical parameters compared to conventional gas chromatography mass spectrometry (GC-MS) method commonly used for ethyl carbamate analysis. DI-ESI-MS/MS method requires just a fast step sample clean up and presents consistent values for the limit of detection (LOD 48.0 μg L-1) and limit of quantification (LOQ 160.0 μg L-1). Furthermore, the recoveries obtained were close to 100%, with relative standard deviations below 10% of sample certificates.

Abstract The objective of this study is to assess, in zebrafish, the effects of combining linseed oil (LO) and clove leaf essential oil (CLEO) on the incorporation of fatty acids in the muscle, oxidative markers, lipid peroxidation and expression of the PPAR-α (Peroxisome Proliferator-Activated Receptor-α) and the SREBP-2 (Sterol Regulatory Element Binding Protein-2) genes. Six diets were prepared, containing combinations of LO (3, 6 and 9%) and CLEO (0.5 and 1%): 3% LO + 0.5% CLEO; 3% LO + 1% CLEO; 6% LO + 0.5% CLEO; 6% LO + 1% CLEO; 9% LO + 0.5% CLEO; 9% LO + 1% CLEO. Results showed increase in the incorporation of n-3 fatty acids in the muscle concomitantly with the addition of LO and CLEO. The activities of superoxide dismutase and catalase were reduced and the glutathione content had increased. Lipid peroxidation was lower in the treatment with 1% CLEO, regardless of LO content. The expression of the PPAR-α and the SREBP-2 genes was higher in animals fed 9% LO + 0.5% CLEO. Therefore, for a greater incorporation and protection against the oxidative damages of n-3 fatty acids, a combined use of 9% LO with 0.5% CLEO is recommended for zebrafish.

Acerola is a tropical fruit with a large industrial and commercial appeal due to its organoleptic qualities and bioactive compound-rich nature. Thus, as bioactive compounds (BC) stability is of great interest in the food industry, assessment of preserving techniques to prolong shelf life has become imperative. Hence, the purpose of this study was to evaluate how storage affects BC conservation in microencapsulated and lyophilized acerola pulps over 180 days. For this matter, antioxidant tests, physical-chemical analyzes, and vitamin C analysis by mass spectrometry were performed. Results indicated that microencapsulation better preserved the antioxidants in acerola pulp compared to the other preservation technologies employed. This is due to the greater BC concentration in the microencapsulated, as well as the pH reduction. Furthermore, over 180 days, microencapsulation better preserved the target compounds in acerola pulp compared to lyophilization, as evidenced by the superior content of BC in the former treatment, making it an appealing option for the food sector.

The present work intends to obtain and characterize a milk by-product: the human whey (HW), in order to avoid the excessive disposal of human milk (HM). The characterization was performed through analyzes of the chemical composition and fatty acids (FAs) and the triacylglycerol (TAG) lipid profile. The results indicated that the chemical composition altered significantly after the HW obtained, except for the percentage of ash and carbohydrates. About the FA composition, it was observed that strictly essential FA, essential FA and other FAs found in HM remained present in HW. For the nutritional lipids quality, the atherogenicity and the thrombogenicity indices presented desirable values, and the TAGs lipid profile revealed a variation in the analyzed samples. Therefore, it can be concluded that the characterized HW has potential for application in isolated form or to be used as an ingredient in other foods.

Rosemary (Rosmarinus officinalis L.) is known for its bioactive compounds with high antioxidant potential and pharmacological properties, such as antibacterial, antidepressant and anti-inflammatory. These properties are attributed to the presence of (poly)phenolic compounds. In the literature there is no extraction of these compounds with a totally non-toxic solvent, capable of applying the extract directly to the food. This work aimed to optimize the extraction conditions of bioactive compounds from the rosemary leaves using water as solvent. According to the analysis of variance parameters, a cubic model of high order of significance was obtained with adjusted R2 (R squared) > 0.947. The optimal conditions of the antioxidant potential for conventional and ultrasonic agitation were: temperature 70 °C, 30 min of extraction and the solvent/solute ratio of 25, resulting in an antioxidant potential of 6861 and 7126 µmol L−1 Trolox, respectively. The electrospray ionization mass spectrometry (ESI(−)-MS/MS) analysis showed the presence of antioxidant compounds such as: carnosol (m/z 329.20), rosmanol (m/z 345.03) and rosmarinic (m/z359.14) acids. The response surface methodology evaluated the influence of the main parameters of the bioactive compounds extraction from rosemary using only water as solvent, in addition to the use of less time and sample mass, resulting in lower cost.

Considering the increasing number of low cost vegetable oil product adulterations, it is necessary to assess the authenticity of the lipid sources used in the dog food manufacture, consequently different brands and classifications of feed were analyzed to verify the product authenticity by gas chromatography (GC) with flame ionization detector (FID) and by electrospray ionization mass spectrometry (ESI-MS). Fatty acid (FA) composition analysis was performed to compare the FAs amount in samples with the respective guarantee levels stated by the manufacturers on its product label. Gas chromatography with flame ionization detector (GC-FID) results for omega-3 and 6 percentages are within the limits presented by each manufacturer, while the timnodonic + cervonic acids amount information presented on feed sample labels is not in accordance with GC-FID results. Consequently, the samples were analyzed by ESI-MS, the results exposed the chicken oil presence in the feed and eicosapentaenoic (EPA) + docosahexaenoic (DHA) acids absence, since no lipid profiles similar to fish oils or triacylglycerols (TAGs) containing these two FAs were found. Thus, the information presented on labels are in disagreement with the results obtained both by GC-FID FA composition analysis and by ESI-MS lipid profile analysis. Principal component analysis (PCA) confirmed that the main contribution was from FAs found by GC-FID.

This paper describes the monitoring of ethyl carbamate concentration in sugar cane spirit from industrial distilleries in Brazil. In total, 18 distilleries from Minas Gerais and São Paulo states were evaluated, with, a total of 336 samples from August 2017 to August 2019. The ethyl carbamate was analyzed using a previously validated mass spectrometric method. Analytical curves presented coefficient of determination (R2) values higher than 0.99, and quality control samples showed a relative standard deviation (RSD) below 9%. Concentrations of ethyl carbamate ranged from not detected to 1608 µg L-1, with mean values of 294.2, 280.7 and 230.0 µg L-1 in 2017, 2018, and 2019, respectively. On average, 46, 44 and 69% of samples presented levels of ethyl carbamate below 210 µg L-1. A variety of factors may have led to distillery A having a low level (ca. 115 µg L-1) of ethyl carbamate, including controlled temperature, yeast strain, post-harvesting quality, sugar cane variety choice, and the treatment process on the sugar cane juice, which goes towards the addition of Ca(OH)2, heating and freezing. These results showed the importance of internal quality control, and that sugar cane juice treatment may be a way to decrease ethyl carbamate in the distilleries.

In order to provide an effective and environmentally correct alternative for oil extraction, subcritical n-propane was used under different temperature and pressure conditions to obtain Brazil nut oil. The composition of the oil was determined and compared to the oils obtained by conventional methods. The result of the extraction yield obtained using subcritical fluid extraction (SFE) at 60 ºC, 6 MPa and granulometry < 1.40 mm (63.13%) presented minor differences to the yield obtained by Soxhlet extraction (SE) (68.44%) and Bligh and Dyer extraction (BD) (59.54%). The composition in fatty acids was similar regardless of the method of extraction used. Oxidized triacylglycerols (TAGs) were found in the oils extracted by SE and BD while they were not detected in the oils extracted by SFE. The quantity of bioactive compounds was higher in the oils obtained by SFE. Thus, the SFE using n-propane preserves the nutritional characteristics and lipophilic components of the oil, besides improving the availability of bioactive compounds from an effective “green extraction” without the use of toxic solvents.