The growing demand in natural matrices that represent a source of dietary and nutraceutical molecules has led to an increasing interest in Cannabis sativa, considered to be a multipurpose, sustainable crop. Particularly, the considerable content in essential fatty acids (FAs) makes its derived-products useful food ingredients in the formulation of dietary supplements. In this research, the FA and triacylglycerol (TAG) composition of hempseed oils and flours were investigated using gas chromatography coupled to mass spectrometry and flame ionization detection as well as liquid chromatography coupled to mass spectrometry (LC-MS), respectively. Furthermore, a recently introduced linear retention index (LRI) approach in LC was successfully employed as a useful tool for the reliable identification of TAG species. A total of 30 FAs and 62 glycerolipids were positively identified in the investigated samples. Relative quantitative analyses confirmed linoleic acid as the most abundant component (50–55%). A favorable omega6/omega3 ratio was also measured in hemp-derived products, with the α-linolenic acid around 12–14%. Whereas, γ-linolenic acid was found to be higher than 1.70%. These results confirm the great value of Cannabis sativa as a source of valuable lipids, and the further improvement of the LRI system paves the way for the automatization of the identification process in LC.
This work aimed to investigate Sinapis pubescens subsp. pubescens spontaneously grown in Sicily (Italy) as new potential source of active metabolites; specifically, a comparative study on leaf, flower, and stem hydroalcoholic extracts was performed. Polyphenols were quantitatively determined by spectrophotometric methods and characterized by HPLC‐PDA/ESI‐MS; a total of 55 polyphenolic compounds were identified, highlighting considerably different qualitative‐quantitative profiles. The extracts showed antioxidant activity, evaluated by in vitro assays; particularly, the leaf extract displayed the best radical scavenging activity (DPPH test) and reducing power, while the flower extract showed the greatest chelating activity. The antimicrobial properties of the extracts were investigated against bacteria and yeasts by standard methods; no antimicrobial activity was found against the strains tested. The extracts resulted to be non‐toxic after preliminary toxicity evaluation by the Artemia salina lethality bioassay. The aerial parts of S. pubescens subsp. pubescens proved to be valuable sources of antioxidants for pharmaceutical and nutraceutical applications.
Triacylglycerols (TAGs), as the main components of edible oils and animal fats, are responsible for the nutritional value, organoleptic features and technological properties of foods; each lipid matrix shows a unique TAG profile which can serve as fingerprint to ensure the quality and authenticity of food products. The high complexity of many foodstuffs often makes untargeted elucidation of TAG components a challenging task; thus, more efficient separation techniques may be mandatory. In this research, the TAG profile of a borage (Borago officinalis) seed oil was obtained by two-dimensional comprehensive liquid chromatography (LC×LC), by the coupling of silver thiolate and octadecylsilica monodisperse materials. A total 94 TAG compounds were identified by ion trap-time of flight detection, using atmospheric pressure ionization, with the degree of unsaturation varying from 0 to 9, and partition values ranging from 36 to 56. The group-type separation afforded by this analytical approach may be useful to quickly fingerprint TAG components of oil samples.
Recently, our research team has started a study on Brassica fruticulosa subsp. fruticulosa, an edible plant traditionally used to treat various ailments, little investigated to date. Good in vitro antioxidant properties were highlighted for the leaf hydroalcoholic extract, with the secondary higher than the primary ones. In continuation of the ongoing research, this work was designed to elucidate the antioxidant properties of the phenolic compounds contained in the extract. For this purpose, a phenolic-rich ethyl acetate fraction (Bff-EAF) was obtained from the crude extract by liquid–liquid extraction. The phenolic composition was characterized by HPLC-PDA/ESI-MS analysis and the antioxidant potential was investigated by different in vitro methods. Furthermore, the cytotoxic properties were evaluated by MTT, LDH and ROS determinations on human colorectal epithelial adenocarcinoma cells (CaCo-2) and human normal fibroblasts (HFF-1). Twenty phenolic compounds (flavonoid and phenolic acid derivatives) were identified in Bff-EAF. The fraction exhibited good radical scavenging activity in the DPPH test (IC50 = 0.81 ± 0.02 mg/mL), and moderate reducing power (ASE/mL = 13.10 ± 0.94) and chelating properties (IC50 = 2.27 ± 0.18 mg/mL), contrary to what previously observed for the crude extract. Bff-EAF reduced in a dose-dependent manner CaCo-2 cell proliferation after 72 h of treatment. This effect was accompanied by the destabilization of the cellular redox state due to the antioxidant and pro-oxidant activities displayed by the fraction at lower and higher concentrations. No cytotoxic effect was observed on HFF-1 fibroblasts, used as control cell line.
Supercritical fluid chromatography (SFC) has witnessed a resurge of interest in the last decade, motivated by substantial progress in hardware capabilities and the development of specifically tailored packing materials. Meanwhile, the technique has been transitioning to the use of mobile phases in which an organic co-solvent is mixed to carbon dioxide under subcritical conditions (subFC). The use of a mobile phase modifier will also affect the selectivity, and extend the range of SFC-amenable compounds, including lipids. In this research, a subFC method was developed for the separation of triacylglycerols (TAGs) in edible oils of vegetable origin, namely borage, corn, hazelnut, olive, palm, peanut, and soybean oil. For all the samples investigated, elution of the TAG species was achieved within 8 min, the only exception being borage oil (14 min run), characterized by TAGs spanning in a wide range of partition number (PN 36–56), as constituted by fatty acids differing for alkyl chain lengths (CN 14–24), and degree of unsaturation (DB 0–9). The coupling to mass spectrometry (MS) detection allowed for the average parameters of fatty acid composition to be derived in the oil TAG constituents. A total of 121 TAGs were identified by subFC-MS, with reduced analysis time and solvent consumption (1.5 mL per analysis) compared to common chromatographic approaches. Key features of the method developed hereby are low toxicity, costs, and environmental impact. Notably, the achieved separations were conducted at room temperature, which is beneficial in terms of column life.