Antonella Cavazza

Characterization of 12 Capsicum varieties by evaluation of their carotenoid profile and pungency determination.

In this research 12 different varieties of Capsicum cultivars belonging to three species (Capsicum chinense, Capsicum annuum, Capsicum frutescens) and of various colour, shape, and dimension have been characterised by their carotenoids and capsaicinoids content. The berries were cultivated in the region Emilia-Romagna, in Northern Italy. The native carotenoid composition was directly investigated by an HPLC-DAD-APCI-MS methodology, for the first time. In total, 52 carotenoids have been identified and considerable variation in carotenoid composition was observed among the various cultivars investigated. Among the cultivars with red colour, some Habanero, Naga morich and Sinpezon showed an high β-carotene content, whereas Serrano, Tabasco and Jalapeno showed an high capsanthin content and the absence of β-carotene. Habanero golden and Scotch Bonnet showed a high lutein, α-carotene and β-carotene amounts, and Habanero orange was rich in antheraxanthin, capsanthin and zeaxanthin. Cis-cryptocapsin was present in high amount in Habanero chocolate. The qualitative and quantitative determination of the capsaicinoids, alkaloids responsible for the pungency level, has also been estimated by a validated chromatographic procedure (HPLC-DAD) after a preliminary drying step and an opportune extraction procedure. Results have also been expressed in Scoville units. Dry matter and water activity have also been established on the fresh berries. The dried peppers of each variety were then submitted to the evaluation of the total nitrogen content, measured by a Dumas system, permitting to provide information on the protein content that was found to be in the range between 7 and 16%.

High-Performance Anion-Exchange Chromatography Coupled with Pulsed Electrochemical Detection as a Powerful Tool to Evaluate Carbohydrates of Food Interest: Principles and Applications

Specific HPLC approaches are essential for carbohydrate characterization in food products. Carbohydrates are weak acids with pKa values in the range 12–14 and, consequently, at high pH can be transformed into oxyanions, and can be readily separated using highly efficient anion-exchange columns. Electrochemical detection in HPLC has been proven to be a powerful analytical technique for the determination of compounds containing electroactive groups; pulsed amperometric detection of carbohydrates is favourably performed by taking advantage of their electrocatalytic oxidation mechanism at a gold working electrode in a basic media. High-performance Anion Exchange Chromatography (HPAEC) at high pH coupled with pulsed electrochemical detection (PED) is one of the most useful techniques for carbohydrate determination either for routine monitoring or research application. This technique has been of a great impact on the analysis of oligo- and polysaccharides. The compatibility of electrochemical detection with gradient elution, coupled with the high selectivity of the anion-exchange stationary phases, allows mixtures of simple sugars, oligo- and polysaccharides to be separated with high resolution in a single run. A few reviews have been written on HPAEC-PED of carbohydrates of food interest in the last years. In this paper the recent developments in this field are examined.

High-performance liquid chromatographic phenolic compound fingerprint for authenticity assessment of honey.

BACKGROUND Phenolic compound profiles of 20 honeys of different botanical origin (eucalyptus, citrus, chestnut and linden) were obtained by high-performance liquid chromatography with ultraviolet detection after solid phase extraction, in order to evaluate the effectiveness of the fingerprint method for monofloral honey discrimination. RESULTS A total of 58 peaks were detected at λ = 280 nm. Distinctive phenolic compound profiles were obtained in which both the nature and the relative amount of the detected compounds were characteristic for different botanical source honeys. In order to detect sample groupings, chromatographic peak areas were submitted to principal component analysis. Then linear discriminant analysis was carried out on the first three principal components. In addition, linear discriminant analysis was carried out on the 58 variables, allowing the selection of five variables able to discriminate honeys of different botanical origin. CONCLUSION The chemometric evaluation of the phenolic compound profiles yielded classification models able to group honey samples according to their floral source with an excellent degree of agreement. The main advantage of the fingerprint approach with respect to traditional methods is that it does not require time-consuming identification and quantification of the analytes. The method proved to be effective for the assessment of honey authenticity.

Evaluation of Fructooligosaccharides and Inulins as Potentially Health Benefiting Food Ingredients by HPAEC-PED and MALDI-TOF MS

This paper describes the complementarity of high-performance anion exchange chromatography coupled with pulsed electrochemical detection (HPAEC-PED) and matrix-assisted laser desorption/ionization mass spectrometry (MALDI-TOF-MS) to evaluate commercial available fructans (fructooligosaccharides (FOS) and inulins), having different degrees of polymerization (DP) which are usually employed by food industry as functional ingredients either for their prebiotic properties or as a fat replacer, giving a fat-like mouth feel and texture. The developed HPAEC-PED methods are able to analyze FOS (fructans with DP 3–10) and inulins (DP ranging from 3 to 80) with a good resolution and relatively short retention times to evaluate structural differences between fructooligosaccharide and inulins and the possible presence of inulooligosaccharides as well as of branching. To characterize FOS and inulin at different degrees of polymerization and to assure correct molecular assignment, MALDI-TOF MS analysis was also investigated. The 2,5-dihydroxy benzoic acid (2,5-DHB) was found to be the best matrix for FOS analysis as Actilight and Raftilose P95 products, while 3-aminoquinoline (3-AQ) seems to be the best matrix for inulin with higher DP. The applicability of the optimized methods to the identification and determination of FOS contained in a symbiotic milk as well as a type of inulin added as functional ingredient to a cooked ham is demonstrated.

Determination of furosine in food products by capillary zone electrophoresis-tandem mass spectrometry

A new method for qualitative and quantitative analysis of furosine in food products by capillary electrophoresis coupled to tandem mass spectrometry (CE‐MS2) has been optimized and validated. In analytical conditions, the pH value of the run buffer was similar to that of the hydrolyzed samples, which helps in avoiding interactions of the analyte with silanol groups of the inner wall of the fused silica capillary. In all previous CE methods proposed in literature, no SPE treatment has been used. The method has been applied to the analysis of food products, such as flour, having low amounts of furosine. Flour samples of different origin (wheat, chestnut, lupin, einkorn, chickpeas) have been investigated. Different food products such as pasta, milk, and tigelle bread (a typical Italian unleavened bread) were also analyzed. Some of the samples have also been analyzed by reversed‐phase HPLC, and when compared to CE‐MS, data obtained showed good agreement. CE‐MS, in comparison to HPLC, showed advantages in terms of time of analysis and cost. The validation procedure provided good values for LOD and LOQ (respectively 0.07 and 0.25 mg L−1), recovery (77 and 97%), and precision investigated in terms of intraday repeatability (RSD%: 4–6% for peak areas; 1–2% for migration times) and intermediate precision (below 16% for peak areas, and below 7% for migration times). Therefore, the technique reported can be proposed as a powerful analytical method and a valid alternative to common traditional analytical techniques.

On the genuineness of citrus essential oils. Part LIII. Determination of the composition of the oxygen heterocyclic fraction of lemon essential oils (Citrus limon (L.) Burm. F.) by normal-phase high performance liquid chromatography

The oxygen heterocyclic fraction of cold-pressed lemon essential oils has been studied by normal-phase HPLC. The components of the fraction have been isolated by column chromatography, TLC and semi-preparative HPLC with recycle. The identification of the isolated components has been carried out by 1H-NMR and mass spectrometry. Three coumarins (5-geranyloxy-7-methoxycoumarin, citropten, 5-isopentenyloxy-7-methoxycoumarin) and ten psoralens (bergamottin, 8-geranyloxypsoralen, oxypeucedanin, byakangelicol, oxypeucedanin hydrate, byakangelicin, imperatorin, phellopterin, isoimperatorin, 5-isopent-2′-enyloxy-8-(2′,3′-epoxyisopentyloxy)-psoralen) have been isolated and identified. The main components were bergamottin (160–291 mg/100 g of oil) and 5-geranyloxy-7-methoxycoumarin (180–250 mg/100 g of oil). Moreover, herniarin, a coumarin characteristic of lime essential oil, has been detected. Herniarin had been reported previously in essential oils obtained from Citrus limon L. var. Eureka.

Targeted and untargeted data-dependent experiments for characterization of polycarbonate food-contact plastics by ultra high performance chromatography coupled to quadrupole orbitrap tandem mass spectrometry

Materials that come in contact with foods are potential sources of chemical food contamination. Consequently, characterization of their composition is of paramount importance considering the possible occurrence of several unknown molecules such as non-intentionally added substance (NIAS), residual monomers, degradation products, plastic additives and organic colorants. Previous studies concerning the characterization in terms of composition are focalized in the recognition of additives. To the best authors knowledge there are no scientific data about the composition of a plastic material in terms of colorants. In this work, an analytical method employing capillary ultra high-performance liquid chromatography and electrospray ionization quadrupole orbitrap high-resolution mass spectrometry (UHPLC-ESI Q-orbitrap) was exploited for characterization of polycarbonate for food contact material. Data-dependent experiments for targeted and untargeted analysis were employed after a total dissolution of polycarbonate samples and extraction of its components. The presence of common additives such as antioxidants and UV absorbers was confirmed by targeted analysis, while, the untargeted approach combined with the high mass accuracy of orbitrap technology allowed to identify for the first time some polycarbonate degradation products and the organic dyes effectively used for the coloration of plastic objects intended to come in contact with food. The present study shows the high potential of this technique in the field of material characterization aimed at food safety evaluation.

Capillary electrophoresis coupled with mass spectrometry for the evaluation of substance P enzymatic degradation by SaOS-2 human osteosarcoma

A new analytical method for the detection and the quantitative evaluation of the undecapeptide substance P by capillary electrophoresis coupled with ion trap mass spectrometry (CE-MS) by a co-axial sheath liquid interface has been developed. Conditions of analysis employed an acidic buffer and a 60 cm fused silica capillary installed by overcoming the UV window position, thus allowing to perform the analysis in a brief time. The method has been applied to the evaluation of substance P enzymatic hydrolysis during incubation with the human osteosarcoma SaOS-2 cell line. The analysis of amino acids derived from the cleavage of substance P has been also carried out simultaneously under the same electrophoretic conditions allowing the description of a kinetic of amino acid formation, parallel with substance P disappearance. The amounts of intact substance P and of free amino acids were monitored along 600 s of incubation time. A steady decrease of substance P as function of reaction time was observed. Peptides half-life was found to be about 4.3s, indicating an extremely fast hydrolysis in the presence of the SaOS-2 cells. Proline, phenilalanine and methionine were the predominant free amino acids recorded. Obtained results lead to hypothesize the occurrence of endopeptidases activity, followed by aminopeptidases responsible for the release of free amino acids originated after primary bond cleavage.

An innovative method based on quick, easy, cheap, effective, rugged, and safe extraction coupled to desorption electrospray ionization-high resolution mass spectrometry for screening the presence of paralytic shellfish toxins in clams

The capabilities of desorption electrospray ionization-high resolution mass spectrometry (DESI-HRMS) were tested for screening the presence of some paralytic shellfish toxins in clams. A quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach is proposed for sample clean-up. QuEChERS extraction was optimized by using a full factorial design followed by the multicriteria method of the desirability functions. Quantitation limits in the microgram per kilogram range proved reliability of the method for the detection of the investigated toxins in accordance to the rules laid down by European legislation. The optimized QuEChERS-DESI-HRMS based-method allowed for a rapid reliable screening of the investigated compounds at levels of interest, thus being useful for high-throughput analyses.

Uruguayan Essential Oils. Part V. Composition of Bergamot Oil

Abstract The analysis of industrial and laboratory-prepared bergamot oils produced in Uruguay during the 1995 production season was carried out by GC and GC/MS. The composition of the Uruguayan bergamot oils were compared with those of Italian bergamot oils. They were found to be very similar; however, they could be differentiated from their psoralen and coumarin contents. The enantiomeric ratio of linalool and linalyl acetate was also studied by GC using a β-cyclodextrin column. The results were similar to that found in Italian oils.