Sunflower oil has several properties that are valuable to the human skin and health; however, they are target of adulterations. In this study, in order to evaluate the authenticity of edible and cosmetics based on sunflower oils, the triacylglycerol (TAG) profiles using direct infusion electrospray ionization mass spectrometry (ESI-MS), the fatty acid (FA) composition by gas chromatography with flame ionization detection (GC-FID) and principal component analysis, of seven commercial samples were determined and the results obtained were compared with the pure sunflower and soybean oils. Of the seven brands analyzed, just one sample presented only sunflower oil in its composition; two stated in the label soybean addition; and four did not present the real composition of the product in the label. Therefore, GC-FID and ESI-MS analysis in conjunction with principal component analysis (PCA) demonstrated that they are complementary techniques and could be applied in food industries to assess the quality of vegetable oils, since results showed the need for stricter quality control for this product.

Human milk (HM) lipids provide about 50% energy and facilitate the transport and absorption of fat-soluble vitamins for infants, but their composition should be studied when the milk is processed. This study evaluated the lipid quality of lyophilized and vacuum-packed colostrum (C), transitional (T), and mature (M) HM for a period of 1, 30, 60, 90, 120, 150, and 180 days of storage at –18 ºC. From the acidity (ºDornic), lipid content, and fatty acid (FA) composition results, no significant differences in the analyzed period were observed. The relative percentage of major triacylglycerols (TAG) of the HM was not altered, showing that the lyophilization process in HM is a good alternative that could be applied in human milk banks (HMB), increasing HM preservation and facilitating its transport and storage.

Coconut oil has several domestic uses and health benefits, which can be used in food, pharmaceuticals and cosmetics products. However, it has been the target of adulteration with lower price oils and fats, such as soybean oil. In this study, a fast, easy and simple methodology was used to detect low quantities of intentionally adulterated coconut oil with soybean oil by direct infusion electrospray ionization mass spectrometry (ESI-MS) at different levels (0, 2, 5, 10, 15, 20, 30, 50, 70 and 100%). In the oil industry, intentional adulterations usually occur with the addition of low quantities of soybean oil to coconut oil. Therefore, the suggested ESI-MS method is promising for routine analysis to guarantee the quality control of coconut oil since it is possible to detect adulteration with a minimal of 2% soybean oil addition.

Vegetable oils have properties that are beneficial to the human skin, and so, they are being used increasingly as ingredients of many cosmetic preparations; however, they are targets of adulteration. This study will evaluate the authenticity of Brazilian cosmetics based on vegetable oils (sesame, peanut, sunflower, and almonds) to determine the composition of fatty acids by gas chromatography with flame ionization detection (GC-FID) and the percentage of fatty acids in conjunction with chemometric treatments (principal component analysis), and lipid profiles using direct infusion electrospray ionization mass spectrometry (ESI-MS). The results obtained were compared with the respective pure vegetable oils. Of the seven brands analyzed, three were revealed as authentic, three were found to be adulterated with the addition of large amounts of soybean oil, and one showed no vegetable oils. These results demonstrate the relevance of quality control for cosmetics based on vegetable oils, which are more susceptible to adulteration owing to their higher cost when compared with vegetable oils such as soybean.

In this study, a rapid and simple analytical method was proposed, based on protein precipitation as sample preparation for simultaneous determination of tetracycline, oxytetracycline, penicillin G and ceftiofur in raw milk by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The method was applied to raw milk samples from dairy cows medicated with tetracycline for subclinical mastitis. Samples were collected from the adjacent teat to the teat treated with tetracycline of eight different cows at 24, 48, 72 and 96 h after treatment. The limits of quantification of the proposed method ranged between 1 and 5 ng g-1 and limits of detection ranged between 0.1 and 0.5 ng g-1. The recoveries ranged from 61 to 111% and the linear range was 1 to 2064 ng g-1 for tetracycline and oxytetracycline, and 5 to 2064 ng g-1 for penicillin G and ceftiofur. Approximately 75 and 63% of the treated animals revealed more tetracycline than legally recommended at 72 and 96 h since last treatment, respectively.

The Mehlich-1 extractor is routinely used to evaluate the bioavailability of metals in soil since it has a high closeness between the amount of these elements absorbed by the plants and those available in soil, as well as being simple and practical to use. Thus, the aim of this work was to improve (optimize) a Mehlich-1 extraction method for evaluating the availability of Cu, Zn, Mn, Ni, Cr and Cd in soil using Box-Behnken type response surface method (RSM). After optimizing the soil amount, Mehlich-1 extractor volume and stirring time, the validation of the newly developed method was performed by evaluating the following parameters: matrix adjustment, linearity, linear range, limits of detection (LOD) and of quantification (LOQ), precision and accuracy. The analytical method proposed by this study can be routinely employed for the evaluation of soil toxicity since it presented advantages such as simplicity, speed and efficacy, as well as being precise and accurate.

The investigation of the distribution of antioxidant compounds between emulsions phases, employing natural sources of these compounds directly in the emulsions, is rarely addressed. The use of ultra performance liquid chromatography coupled to a mass spectrometer (UPLC-MS), combined with accelerated oxidation tests and oxygen radical absorbance capacity method (ORAC), using the fluorescein (FL) decay curve (ORACFL) assay, enable an improved evaluation of the distribution of the antioxidant compounds and their lipid protection abilities. The lipid protection tendency observed was in agreement with the polar paradox theory. The ORACFL results reported here are higher than other reported in the literature, even when performing a sample extraction directly into one of the emulsion phases, thus demonstrating the effectiveness of this direct addition regarding the antioxidant activity. The analysis of the mass spectra of the emulsions enabled to verify the existence and distribution of some phenolic compounds in both phases. The direct extraction in the aqueous and oil phases of the emulsion increased, in a general way, the amount of identified compounds in each phase.

This study evaluated the incorporation of β-carotene, lutein and lycopene into tilapia (genetically improved farmed tilapia, GIFT) fillets supplemented through 0, 20 and 40 days, and their influence on the fatty acid composition and nutritional quality of raw and grilled fillets. A control diet and a diet containing those carotenoids were elaborated with the same lipid source (soybean oil). For carotenoids analysis, the extraction was performed according to the literature, employing acetone and hexane. The relative intensities of m/z ratios of those carotenoids ions were obtained by ultraperformance liquid chromatography-tandem mass spectrometry with chemical ionization at atmospheric pressure (UPLC-APCI MS/MS), and an increase of carotenoid concentration in the supplemented fillets was observed, especially after the grilling process (180 ºC for 15 min). An increase in the concentration of total carotenoids in grilled fillets (75 and 35% higher than raw fillets, for 20 and 40 days of supplementation, respectively, corresponding to 8.32 and 2.42 µg β-carotene g-1 sample) was also observed. Therefore, the carotenoids promoted the stability of lipid oxidation in grilled samples; fact that can be correlated with antioxidant effect of these compounds, it can be also explained by the breakdown of carotenoids physical barrier and the conditions used in the grilling process. Moreover, acceptable n-6/n-3 indices and recommended polyunsaturated fatty acids/saturated fatty acids (PUFA/SFA) values were observed in supplemented fillets. Consequently, lutein, β-carotene and lycopene were considered viable as additive on fish diet, since the supplementation promoted the increase of food quality, even after preparation for consumption.

This work proposed a novel, relatively low-cost and rapid analytical method using microemulsion as sample preparation to determine iron (Fe) in vegetable oils by flame atomic absorption spectrometry technique (FAAS). The vegetable oil microemulsions were obtained by mixing appropriate proportions of the crude and refined vegetable oil, Triton® X-100, 1-propanol and nitric acid 50% (v v-1). Moreover, an external calibration method was established using aqueous Fe standards instead of expensive and unstable organometallic standards. The limits of detection and quantification were 0.40 and 1.3 mg kg-1 of oil, respectively. The accuracy was checked by recovery studies (with recoveries ranging 84-105%) and by Fe determination in digested vegetable oil samples by inductively coupled plasma optical emission spectrometry (ICP OES) as comparative procedure. The proposed analytical method was efficient to determine Fe in crude and refined vegetable oils from various vegetable sources, besides being suitable for routine analyses due to its simplicity.

Omega-3 fish oil supplements are widely consumed as source of eicosapentaenoic (EPA) and docosahexaenoic (DHA) acids, presenting beneficial effects on human health. This study aimed to evaluate fifteen brands of omega-3 fish oil supplements available in Brazilian market in order to estimate the Brazilian reality regarding those supplements. Twelve fatty acids were quantified by gas chromatography with a flame ionization detector (GC-FID), and lipid profile were obtained via mass spectrometry fingerprinting using direct electrospray ionization mass spectrometry (ESI-MS) to assess the form in which fatty acids are present as well as the possible fraud existence. Among all analyzed samples, thirteen brands were revealed as EPA and DHA sources (90.2-440.3 and 77.8-302.3 mg g-1lipid, respectively) in triacylglycerols (TAG) or ethyl esters (EE) form. However, two brands were discovered with addition of large amounts of soybean oil, leading the final consumer to ingest this low-cost oil believing that they are consuming adequate doses of EPA and DHA.