Target analysis and retrospective screening of contaminants in ready-to-eat cooked ham samples through UHPLC-Q-Orbitrap HRMS.

The use of veterinary drugs (VDs) is widely administered to animals for both therapeutic and prophylactic purposes. However, their improper use may involve their occurrence in the final products intended for human consumption. In this scientific work, a method for the investigation of target (n = 30) VDs residues and retrospective suspect screening followed by confirmation using analytical standards of others 38 contaminants in ready-to-eat cooked ham by ultra-high performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was developed. The extraction was performed based on the QuEChERS approach and validated in accordance with the European Regulation 2021/808. The application of the in-house validated method to ready-to-eat cooked ham showed the occurrence of fourteen VDs residues. Despite the important incidence, the concentration levels found were below the maximum residue limits set for VDs in porcine muscle, except for colchicine. Constant monitoring of animals derived food is strongly recommended to ensure the food safety of consumers.

Analysis of Polyphenolic Compounds in Water-Based Extracts of Vicia faba L.: A Potential Innovative Source of Nutraceutical Ingredients.

The water-based extract of broad bean hulls contains several bioactive molecules, including polyphenols well-known to exert antioxidant activity, which could justify its use in nutraceutical formulations. Hence, the current investigation aimed to establish the polyphenolic profile of water-based extracts from broad bean hulls through UHPLC-Q-Orbitrap HRMS analysis. The findings highlighted that p-coumaric acid, chlorogenic acid, and epicatechin were the most common compounds found in the tested extracts, being quantified at a mean concentration of 42.1, 32.6, and 31.2 mg/100 g, respectively. Moreover, broad bean hull extracts were encapsulated into a nutraceutical formulation, after which the antioxidant properties and the bioaccessibility of phenolic compounds during the simulated gastrointestinal (GI) process were investigated and compared with the digested non-encapsulated extract. The data highlighted that following the GI process, the capsules were able to preserve active compounds from the adverse effects of digestion, resulting in a greater antioxidant capacity and polyphenol bioaccessibility in the duodenal and colonic phases, compared with the non-encapsulated extract. Our results showed that the water extract from broad bean hulls may be considered a valuable source of natural polyphenolic compounds; in addition, the use of a gastric-resistant capsule could be a suitable alternative to transport these bioactive compounds to the target tissues.

Bioaccessibility and Antioxidant Capacity of Bioactive Compounds From Various Typologies of Canned Tomatoes.

Tomato (Solanum lycopersicum L.) is one of the most consumed vegetables in the world; it contains high amounts of antioxidant phytochemicals and essential nutrients. Although it is commonly consumed fresh, more than 80% of its consumption derives from processed products. Since limited information on changes in the bioaccessibility of bioactive compounds during gastrointestinal digestion was reported, this current study aimed to monitor the antioxidant activity, total polyphenolic and carotenoid content, and bioaccessibility during in vitro gastrointestinal digestion of different typologies (n = 7) of canned tomatoes. A comprehensive evaluation of the polyphenolic profile of digested and not digested samples was ascertained by ultra-high-performance liquid chromatography combined with high-resolution Orbitrap mass spectrometry. The results highlighted a considerable content of rutin (1.191-9.516 mg/100 g), naringenin (0.359-1.452 mg/100 g), chlorogenic acid (1.857-11.236 mg/100 g), and lycopene (50.894-222.061 mg/kg) in the analyzed matrices. After in vitro gastrointestinal digestion, large variability, losses and low recovery were recorded. An appreciable percentage of rutin (30.7%), naringenin (29.6%), chlorogenic acid (25.8%), and lycopene (varied between 9.3 and 20%) remained bioaccessible after the in vitro gastrointestinal digestion. Our study could be a valid support to evaluate which content of bioactive compounds could be really bioaccessible to exercise beneficial effects on human health.

Multiclass and multi-residue screening of mycotoxins, pharmacologically active substances, and pesticides in infant milk formulas through ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry analysis.

Infant milk formulas are designed to substitute human milk when breastfeeding is unavailable. In addition to human milk and milk-derived products, these formulas can be a vehicle of contaminants. In this work, a multiclass method based on the QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach was developed for the simultaneous determination of contaminants (n = 45), including mycotoxins and veterinary drug residues, occurring in infant milk formulas. By using an ultra-high-performance liquid chromatography quadrupole-Orbitrap coupled with high-resolution mass spectrometry analysis (UHPLC-Q-Orbitrap HRMS; Thermo Fisher Scientific), further retrospective analysis of 337 contaminants, including pesticides, was achieved. The method was validated in accordance with European regulations and applied for the analysis of 54 infant milk samples. Risk assessment was also performed. Dexamethasone was detected in 16.6% of samples (range: 0.905-1.131 ng/mL), and procaine benzyl penicillin in 1 sample at a concentration of 0.295 ng/mL. Zearalenone was found in 55.5% of samples (range: 0.133-0.638 ng/mL) and α-zearalenol in 16.6% of samples (range: 1.534-10.408 ng/mL). Up to 49 pesticides, 11 veterinary drug residues, and 5 mycotoxins were tentatively identified via retrospective analysis based on the mass spectral library. These findings highlight the necessity of careful evaluation of contaminants in infant formulas, considering that they are intended for a vulnerable part of the population.

In Vitro Bioaccessibility and Antioxidant Activity of Polyphenolic Compounds from Spent Coffee Grounds-Enriched Cookies.

Spent coffee ground (SCG) is a significant by-product generated by the coffee industry. It is considered a great source of bioactive molecules well-recognized for exerting biological properties. This study aimed to implement SCG in a baked foods, such as cookies (SCGc), to increase their bioactive potential. A comprehensive study of the polyphenolic fraction of the SCG and SCGc using a high-resolution mass spectrometry analysis was performed. Moreover, the polyphenol bioaccessibility and change in antioxidant activity during simulated gastrointestinal digestion (GiD) were assessed. Data showed that SCGc provided 780 mg of melanoidins, 16.2 mg of chlorogenic acid (CGA), 6.5 mg of caffeine, and 0.08 mg of phenolic acids per 100 g of sample. Moreover, the 5-caffeoylquinic acid was the most relevant CGA found in SCG (116.4 mg/100 g) and SCGc (8.2 mg/100 g) samples. The antioxidant activity evaluated through three spectrophotometric tests, and the total phenolic compounds of SCGc samples exhibited significantly higher values than the control samples. Furthermore, during simulated GiD, the highest bioaccessibility of SCGc polyphenols was observed after the colonic stage, suggesting their potential advantages for human health. Therefore, SCG with high content in bioactive molecules could represent an innovative ingredient intended to fortify baked food formulations.

Drupe Characters, Fatty Acids, Polyphenolic and Aromatic Profile of Olive Oil Obtained from "Oliva Bianca", Minor Autochthonous Cultivar of Campania.

Campania, due to its pedo-climatic conditions and to its large varietal heritage, is able to produce oils with high typicity, each different from the other. In this study a "minor" autochthonous cultivar of Campania "Oliva Bianca" was analyzed. In autumn 2020, on drupes from trees belonging to the Campania germplasm collection a varietal characterization through physical, chemical and chromatic parameters at the harvest was carried out. Phenolic compounds profile, fatty acids composition and volatile organic compounds have been investigated in the resulting oil. Quality indices, organoleptic and sensory qualities (panel test) were also determined on the oil. Drupe weight was 4.31 g, flesh/pit ratio was 3.68 and the accumulation of oil content at harvest in drupes was 18.63% FW. The drupes showed high anthocyanins content equal to 116.10 mg/kg. In the oil studied, the secoiridoids represented the 82.25% of total phenolic compounds, the concentration of oleic acid was 74.82% and the most present volatile compound was trans-2-hexenal (72.30%). High secoiridoid derivatives concentrations such as oleuropein (85.93 mg/kg) and ligstroside (122.43 mg/kg) aglycones were showed. This study showed a good content of qualitative and quantitative parameters of "Oliva Bianca" oil and drupe, that can have important beneficial effects on human health.

Assessment of In Vitro Bioaccessibility of Polyphenols from Annurca, Limoncella, Red Delicious, and Golden Delicious Apples Using a Sequential Enzymatic Digestion Model.

Four different varieties of apples have been considered (Limoncella, Annurca, Red Delicious, and Golden Delicious) to estimate the extent of colon polyphenolics release after in vitro sequential enzyme digestion. Since several studies report a positive effect of apple polyphenols in colonic damage, we found of interest to investigate the colon release of polyphenols in different varieties of apples in order to assess their prevention of colonic damage. UHPLC-HRMS analysis and antioxidant activity (ABTS, DPPH, and FRAP assays) were carried out on the apple extracts (peel, flesh, and whole fruit) obtained from not digested samples and on bioaccessible fractions (duodenal and colon bioaccessible fractions) after in vitro digestion. Polyphenolic content and antioxidant activities were found to vary significantly among the tested cultivars with Limoncella showing the highest polyphenol content accompanied by an excellent antioxidant activity in both flesh and whole fruit. The overall trend of soluble antioxidant capacity from the soluble duodenal phase (SDP) and soluble colonic phase (SCP) followed the concentrations of flavanols, procyandinis, and hydroxycinnamic acids under the same digestive steps. Our results highlighted that on average 64.2% of the total soluble antioxidant activity was released in the SCP with Limoncella exhibiting the highest values (82.31, 70.05, and 65.5%, respectively for whole fruit, flesh, and peel). This result suggested that enzymatic treatment with pronase E and viscozyme L, to reproduce biochemical conditions occurring in the colon, is effective for breaking the dietary fiber-polyphenols interactions and for the release of polyphenols which can exercise their beneficial effects in the colon. The beneficial effects related to the Limoncella consumption could thus be of potential great relevance to counteract the adverse effects of pro-oxidant and inflammatory processes on intestinal cells.

Mycotoxin Occurrence and Risk Assessment in Gluten-Free Pasta through UHPLC-Q-Exactive Orbitrap MS.

Celiac disease (CD) is a genetic-based autoimmune disorder which is characterized by inflammation in the small intestinal mucosa due to the intolerance to gluten. Celiac people should consume products without gluten, which are elaborated mainly with maize or other cereals. Contamination of cereals with mycotoxins, such as fumonisins (FBs) and aflatoxins (AFs) is frequently reported worldwide. Therefore, food ingestion is the main source of mycotoxin exposure. A new analytical method was developed and validated for simultaneous analysis of 21 mycotoxins in gluten-free pasta, commonly consumed by celiac population as an alternative to conventional pasta. Ultrahigh-performance liquid chromatography coupled to quadrupole Orbitrap high-resolution mass spectrometry (UHPLC-Q-Exactive Orbitrap MS) was used for analyte separation and detection. The mycotoxins included in this work were those widely reported to occur in cereal samples, namely, ochratoxin-A (OTA), aflatoxins (AFB1, AFB2, AFG1 and AFG2), zearalenone (ZON), deoxynivalenol (DON), 3-acetyl-deoxynivalenol and 15-acetyl-deoxynivalenol (3-AcDON and 15-AcDON, respectively), nivalenol (NIV), neosolaniol (NEO), fusarenone-X, (FUS-X), T-2 toxin (T-2) and HT-2 toxin (HT-2), fumonisin B1 and B2 (FB1 and FB2, respectively), enniatins (ENN A, ENN A1, ENN B and ENN B1) and beauvericin (BEA). The validated method was successfully applied to 84 gluten-free pasta samples collected from several local markets of Campania region (Italy) during September to November 2020 to monitor the occurrence of mycotoxins and to assess the exposure to these food contaminants. A significant number of samples (95%) showed mycotoxin contamination, being Fusarium mycotoxins (FB1, ZON and DON) the most commonly detected ones. Regarding the risk assessment, the higher exposures were obtained for NIV, DON and FB1 for children and teenagers age group which can be explained due to their lower body weight.

Chemical Composition of Green Pea (Pisum sativum L.) Pods Extracts and Their Potential Exploitation as Ingredients in Nutraceutical Formulations.

Agro-industrial wastes contain a large number of important active compounds which can justify their use as innovative ingredients in nutraceutical products. This study aimed to provide a complete analysis of active molecules, namely (poly)phenols in pea pods water-based extracts, through a UHPLC-Q-Orbitrap HRMS methodology. Data showed that 5-caffeoylquinic acid, epicatechin, and hesperidin were the most relevant (poly)phenols found in the assayed extracts, with a mean value of 59.87, 29.46, and 19.94 mg/100 g, respectively. Furthermore, changes in antioxidant capacity and bioaccessibility of total phenolic compounds (TPC) after the simulated gastrointestinal (GI) process were performed using spectrophotometric assays (FRAP, DPPH, ABTS, and TPC by Folin-Ciocalteu). The acid-resistant capsules (ARC) and the non-acid resistant capsules (NARC) containing the pea pod extract underwent simulated GI digestion. The results suggested that the ARC formulations were able to preserve the active compounds along the simulated GI process, highlighting a higher TPC value and antioxidant capacity than the NARC formulations and the not-encapsulated extracts. Hence, the pea pods water-based extracts could be utilized as a potential alternative source of active compounds, and the use of ARC could represent a suitable nutraceutical formulation to vehiculate the active compounds, protecting the chemical and bioactive properties of (poly)phenols.

An Innovative Olive Pâté with Nutraceutical Properties.

Food plays a central role in health, especially through consumption of plant-derived foods. Functional foods, supplements, and nutraceuticals are increasingly entering the market to respond to consumer demand for healthy products. They are foods, supplements, and ingredients which offer health benefits beyond the standard nutritional value. Some benefits are associated with phenolic compounds and phytochemicals with antioxidant properties. An olive pâté (OP) was added with antioxidants derived from olive mill wastewater (OMWW) to obtain a functional product rich in phenolic compounds. The olive pâté is produced from the ground olive pericarp, which shows an excellent natural antioxidant content. The OMWW is a waste product from oil processing, which is also rich in phenolic compounds. The result was a product rich in trans-resveratrol, OH tyrosol, and tyrosol in concentrations such as satisfying the European community's claims regarding the possible antioxidant action on plasma lipids with excellent shelf-life stability. The total phenolic content was assayed by a colorimetric method, the antioxidant activity by the ABTS [(2,2'-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid)] test, the phenolic profile by Q Exactive Orbitrap LC-MS/MS. The shelf-life stability was confirmed by yeast, molds, and total microbial count, pH, and water activity determinations, and the best pasteurization parameters were determined. The palatability was judged as excellent.

Biomonitoring of Enniatin B1 and Its Phase I Metabolites in Human Urine: First Large-Scale Study.

Enniatins (Enns) are mycotoxins produced by Fusarium spp. which are a fungus widely spread throughout cereals and cereal-based products. Among all the identified enniatins, Enn B1 stands as one of the most prevalent analogues in cereals in Europe. Hence, the aim of this study was to evaluate for the first time the presence of Enn B1 and its phase I metabolites in 300 human urine samples using an ultrahigh-performance liquid chromatography high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) methodology. Enn B1 was detected in 94.3% of samples ranging from 0.007 to 0.429 ng/mL (mean value: 0.065 ng/mL). In accordance with previous in vitro and in vivo analysis, hydroxylated metabolites (78.0% samples) and carbonylated metabolites (66.0% samples) were tentatively identified as the major products. Results from this biomonitoring study point to a frequent intake of Enn B1 in the studied population, suggesting that in-depth toxicological studies are needed in order to understand the potential effects in humans.

New Strategies in the Cultivation of Olive Trees and Repercussions on the Nutritional Value of the Extra Virgin Olive Oil.

The health advantages of extra-virgin olive oil (EVOO) are ascribed mainly to the antioxidant ability of the phenolic compounds. Secoiridoids, hydroxytyrosol, tyrosol, phenolic acid, and flavones, are the main nutraceutical substances of EVOO. Applications of beneficial microbes and/or their metabolites impact the plant metabolome. In this study the effects of application of selected Trichoderma strains or their effectors (secondary metabolites) on the phenolic compounds content and antioxidant potential of the EVOOs have been evaluated. For this purpose, Trichoderma virens (strain GV41) and Trichoderma harzianum (strain T22), well-known biocontrol agents, and two their metabolites harzianic acid (HA) and 6-pentyl-α-pyrone (6PP) were been used to treat plants of Olea europaea var. Leccino and var. Carolea. Then the nutraceutical potential of EVOO was evaluated. Total phenolic content was estimated by Folin-Ciocalteau's assay, metabolic profile by High-Resolution Mass spectroscopy (HRMS-Orbitrap), and antioxidant activity by DPPH and ABTS assays. Our results showed that in the cultivation of the olive tree, T22 and its metabolites improve the nutraceutical value of the EVOOs modulating the phenolic profile and improving antioxidants activity.

Analysis of Phenolic Compounds in Commercial Cannabis sativa L. Inflorescences Using UHPLC-Q-Orbitrap HRMS.

Industrial hemp (Cannabis sativa L. Family Cannabaceae) contains a vast number of bioactive relevant compounds, namely polyphenols including flavonoids, phenolic acids, phenol amides, and lignanamides, well known for their therapeutic properties. Nowadays, many polyphenols-containing products made of herbal extracts are marketed, claiming to exert health-promoting effects. In this context, industrial hemp inflorescence may represent an innovative source of bioactive compounds to be used in nutraceutical formulations. The aim of this work was to provide a comprehensive analysis of the polyphenolic fraction contained in polar extracts of four different commercial cultivars (Kompoti, Tiborszallasi, Antal, and Carmagnola Cs) of hemp inflorescences through spectrophotometric (TPC, DPPH tests) and spectrometry measurement (UHPLC-Q-Orbitrap HRMS). Results highlighted a high content of cannflavin A and B in inflorescence analyzed samples, which appear to be cannabis-specific, with a mean value of 61.8 and 84.5 mg/kg, meaning a ten-to-hundred times increase compared to other parts of the plant. Among flavonols, quercetin-3-glucoside reached up to 285.9 mg/kg in the Carmagnola CS cultivar. Catechin and epicatechin were the most representative flavanols, with a mean concentration of 53.3 and 66.2 mg/kg, respectively, for all cultivars. Total polyphenolic content in inflorescence samples was quantified in the range of 10.51 to 52.58 mg GAE/g and free radical-scavenging included in the range from 27.5 to 77.6 mmol trolox/kg. Therefore, C. sativa inflorescence could be considered as a potential novel source of polyphenols intended for nutraceutical formulations.

Target analysis and retrospective screening of mycotoxins and pharmacologically active substances in milk using an ultra-high-performance liquid chromatography/high-resolution mass spectrometry approach.

Milk is a nutritious food suitable for infants and adults, and it plays an important role in the human diet. However, it may also be a vehicle for food contaminants. In this report, we developed a method using ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-Q-Exactive Orbitrap HRMS; Thermo Fisher Scientific, Waltham, MA) for simultaneous identification of target pharmacologically active substances and mycotoxins in milk. We also used the Q-Orbitrap operating in full scan mode to identify other possible drugs and microbial metabolites that occurred in samples. Fifty-six commercially available milk samples from the Italian market were analyzed. Investigated analytes were extracted using a QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach. Method detection and quantification limits and performance criteria set by European regulations were fulfilled. Pharmacologically active substances were detected in 49% of samples (range 0.007-4.53 ng/mL), including nontarget mycotoxins. Retrospective analysis allowed us to identify other antibiotics and pharmacologically active substances, as well as nonregulated fungal/bacterial metabolites at a relatively high incidence. From the obtained values, the need for continuous monitoring of contaminants in the milk production chain is clear. This is the first study to assess the presence of pharmacologically active substances, mycotoxins, and other microbial metabolites in Italian milk samples using the UHPLC-Q-Orbitrap HRMS system.

Red Wine Consumption and Cardiovascular Health.

Wine is a popular alcoholic beverage that has been consumed for hundreds of years. Benefits from moderate alcohol consumption have been widely supported by the scientific literature and, in this line, red wine intake has been related to a lesser risk for coronary heart disease (CHD). Experimental studies and meta-analyses have mainly attributed this outcome to the presence in red wine of a great variety of polyphenolic compounds such as resveratrol, catechin, epicatechin, quercetin, and anthocyanin. Resveratrol is considered the most effective wine compound with respect to the prevention of CHD because of its antioxidant properties. The mechanisms responsible for its putative cardioprotective effects would include changes in lipid profiles, reduction of insulin resistance, and decrease in oxidative stress  of low-density lipoprotein cholesterol (LDL-C). The aim of this review is to summarize the accumulated evidence correlating moderate red wine consumption with prevention of CHD by focusing on the different mechanisms underlying this relationship. Furthermore, the chemistry of wine as well as chemical factors that influence the composition of the bioactive components of red wine are also discussed.

Target Analysis and Retrospective Screening of Multiple Mycotoxins in Pet Food Using UHPLC-Q-Orbitrap HRMS.

A comprehensive strategy combining a quantitative method for 28 mycotoxins and a post-target screening for other 245 fungal and bacterial metabolites in dry pet food samples were developed using an acetonitrile-based extraction and an ultrahigh-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) method. The proposed method showed satisfactory validation results according to Commission Decision 2002/657/EC. Average recoveries from 72 to 108% were obtained for all studied mycotoxins, and the intra-/inter-day precision were below 9 and 14%, respectively. Results showed mycotoxin contamination in 99% of pet food samples (n = 89) at concentrations of up to hundreds µg/kg, with emerging Fusarium mycotoxins being the most commonly detected mycotoxins. All positive samples showed co-occurrence of mycotoxins with the simultaneous presence of up to 16 analytes per sample. In the retrospective screening, up to 54 fungal metabolites were tentatively identified being cyclopiazonic acid, paspalitrem A, fusaric acid, and macrosporin, the most commonly detected analytes.

Fast analysis of polyphenols and alkaloids in cocoa-based products by ultra-high performance liquid chromatography and Orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap-MS/MS).

The cocoa varieties Criollo, Forastero and Trinitario, which have different organoleptic properties, quite often are mixed together in cocoa-based products. The objective of this work was to develop a rapid method for the simultaneous determination of polyphenols (n = 35) and alkaloids (n = 2) in cocoa-based products by using the high throughput advantages provided by the Q Exactive Hybrid Quadrupole-Orbitrap Mass Spectrometer (HRMS). The proposed procedure was optimized and validated in terms of selectivity and specificity (mass accuracy <5 ppm), sensitivity (instrumental limit of detection from 15 to 30 fg), linearity (r2 > 0.990), accuracy (recovery range from 89.1 to 112.4%) and precision (relative standard deviation <10%). The method was applied to 80 cocoa-based samples. Alkaloids represented on average the 57.7% of assayed compounds. Flavanols and procyanidins were the most abundant polyphenols being quantified in a range between 261 and 668 mg/kg and from 127 to 405 mg/g, respectively. Mass equivalents but structural isomers bioflavonoids were characterized by using the HRMS-Orbitrap methodology here developed.

Urinary levels of enniatin B and its phase I metabolites: First human pilot biomonitoring study.

Enniatins (Enns) are mycotoxins produced by Fusarium spp. and are widely distributed contaminants of cereals and derivate products. Among the different identified enniatins, Enn B is the most relevant analogue in cereals in Europe. Therefore, the aim of this study was to investigate for the first time the occurrence of Enn B and Enn B phase I metabolites in 300 human urine samples throughout an ultrahigh-performance liquid chromatography-high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) methodology. Three different sample preparation procedures were evaluated and salting-out liquid-liquid extraction showed satisfactory validation results. Enn B was quantified in 83.7% of samples ranging from 0.006 to 0.391 ng/mL (average content: 0.016 ng/mL). In line with the in vitro observations with human liver microsomes, in the here analyzed samples the Enn B monooxygenated, N-demethylated and dioxygenated metabolites were tentatively found in 87.7%, 96.3% and 6.7% of samples. The data of this pilot biomonitoring survey indicate a frequent intake of enniatins in Italy, supporting further toxicological studies to provide better basis for understanding their potential effects in humans.

Direct determination of 3-chloropropanol esters in edible vegetable oils using high resolution mass spectrometry (HRMS-Orbitrap).

A series of refined edible oils derived from mixed seeds, peanuts, corn, sunflower and palm obtained from the local supermarket were analyzed for their content of 3-MCPD esters. A direct analytical method for the determination of 3-monochloropropane-1,2-diol esters (3-MCPD esters) was applied to investigate the major MCPD esters found in common edible oils; in particular seven types of monoesters and eleven types of diesters were detected. The limits of detection (LODs) for monoesters and diesters of 3-MCPD were in the range of 0.079-12.678 µg kg-1 and 0.033-18.610 µg kg-1 in edible oils, and the ranges of limits of quantitation (LOQs) were 0.979-38.035 µg kg-1 and 0.100-55 µg kg-1, respectively. The recoveries of 3-MCPD esters from oil samples were in the range of 80-100%, with RSD ranging between 1.9 and 11.8%. The concentration levels of total 3-MCPD diesters in vegetable oil samples were in the range from 0.106 up to 3.444 µg g-1 whereas total monoesters ranged from 0.005 up to 1.606 µg g-1.

Multi-Mycotoxin Analysis in Durum Wheat Pasta by Liquid Chromatography Coupled to Quadrupole Orbitrap Mass Spectrometry.

A simple and rapid multi-mycotoxin method for the determination of 17 mycotoxins  simultaneously  is  described  in  the  present  survey  on  durum  and  soft  wheat  pasta  samples.  Mycotoxins included in the study were those mainly reported in cereal samples: ochratoxin-A  (OTA), aflatoxin B1 (AFB1), zearalenone (ZON), deoxynivalenol (DON), 3-and 15-acetyl-deoxynivalenol  (3-AcDON and 15-AcDON), nivalenol (NIV), neosolaniol (NEO), fusarenon-X, (FUS-X), T-2 toxin  (T-2) and HT-2 toxin (HT-2), fumonisin B1 and B2 (FB1 and FB2), and four emerging mycotoxins:  three  enniatins  (ENA,  ENA1,  and  ENB),  and  beauvericin  (BEA).  Twenty-nine  samples  were  analyzed to provide an overview on mycotoxin presence: 27 samples of durum wheat pasta, and  two samples of baby food. Analytical results concluded that trichothecenes showed the highest  incidence, mainly DON, NIV, and HT-2 toxin, followed by ZON and ENB, while NEO, FUS-X, OTA,  AFB1, and FUM were not detected in any sample. The highest contents corresponded to ENB and  ranged from 91.15µg/kg to 710.90 µg/kg.