This review paper focuses on the recent advancements in the large-scale and laboratory-scale isolation, modification, and characterization of novel starches from accessible botanical sources and food wastes. When creating a new starch product, one should consider the different physicochemical changes that may occur. These changes include the course of gelatinization, the formation of starch-lipids and starch-protein complexes, and the origin of resistant starch (RS). This paper informs about the properties of individual starches, including their chemical structure, the size and crystallinity of starch granules, their thermal and pasting properties, their swelling power, and their digestibility; in particular, small starch granules showed unique properties. They can be utilized as fat substitutes in frozen desserts or mayonnaises, in custard due to their smooth texture, in non-food applications in biodegradable plastics, or as adsorbents. The low onset temperature of gelatinization (detected by DSC in acorn starch) is associated with the costs of the industrial processes in terms of energy and time. Starch plays a crucial role in the food industry as a thickening agent. Starches obtained from ulluco, winter squash, bean, pumpkin, quinoa, and sweet potato demonstrate a high peak viscosity (PV), while waxy rice and ginger starches have a low PV. The other analytical methods in the paper include laser diffraction, X-ray diffraction, FTIR, Raman, and NMR spectroscopies. Native, "clean-label" starches from new sources could replace chemically modified starches due to their properties being similar to common commercially modified ones. Human populations, especially in developed countries, suffer from obesity and civilization diseases, a reduction in which would be possible with the help of low-digestible starches. Starch with a high RS content was discovered in gelatinized lily (>50%) and unripe plantains (>25%), while cooked lily starch retained low levels of rapidly digestible starch (20%). Starch from gorgon nut processed at high temperatures has a high proportion of slowly digestible starch. Therefore, one can include these types of starches in a nutritious diet. Interesting industrial materials based on non-traditional starches include biodegradable composites, edible films, and nanomaterials.

• Klíčová slova
• amylose–lipid complexes, edible films, granule size, nanomaterials, resistant starch, starch analyses, temperature of gelatinization,
• Publikační typ
• časopisecké články MeSH
• přehledy MeSH

The distinction of lipid isomers is gaining more attention in lipidomics due to their different biochemical properties in the organism. Herein, we aimed to develop a method for the analysis of monoacylglycerol (MG) and diacylglycerol (DG) enantiomers in biological samples using chiral supercritical fluid chromatography and mass spectrometry (SFC-MS). Amylose-based chiral columns showed a certain degree of separation of MG and DG isomers, but low selectivity for the acylglycerol classes in total lipid extracts, which could not be improved by modifier composition or other chromatographic conditions. The coelution of MG and DG enantiomers with highly concentrated triacylglycerols (TGs) negatively affected their MS determination based on the peak area ratio, therefore the interclass selectivity of chiral SFC was adjusted by coupling with an achiral column. The connection of the amylose tris-(3,5-dimethylphenylcarbamate) chiral column with octadecyl achiral column using a methanol as a modifier provided an excellent interclass separation of acylglycerols with the resolution of 5.53 and 15.17 for oleic acid-based MG/DG and DG/TG classes, respectively. The developed method enabled the determination of MG and DG enantiomers in complex total lipid extracts of biological samples in a 15 min gradient without time-consuming sample prefractionation. Chiral SFC-MS analysis of egg yolk, human plasma, and porcine brain samples showed different ratios of enantiomers, suggesting their unique roles within each sample type.

• Klíčová slova
• Chiral separation, Column coupling, Diacylglycerol, Monoacylglycerol, Selectivity, Supercritical fluid chromatography,
• MeSH
• amylosa chemie   analogy a deriváty   MeSH
• diglyceridy * chemie   analýza   MeSH
• hmotnostní spektrometrie metody   MeSH
• lipidomika metody   MeSH
• monoglyceridy * chemie   analýza   MeSH
• stereoizomerie MeSH
• superkritická fluidní chromatografie * metody   MeSH
• zvířata MeSH
• Check Tag
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• amylosa MeSH
• diglyceridy * MeSH
• monoglyceridy * MeSH

BACKGROUND: Fatty acid esters of hydroxy fatty acids (FAHFAs) are a recently discovered class of endogenous bioactive lipids with promising therapeutic potential for diabetes and inflammation. They represent complex mixtures of different isomers whose biological functions are the subject of investigation. Highly selective methods are required to characterize the composition of enantiomers in biological samples composed of many isobars and regioisomers. We aimed to develop a method for characterizing the enantiomeric composition of FAHFAs in biological samples using supercritical fluid chromatography-mass spectrometry (SFC-MS). RESULTS: The influence of key chromatographic parameters, such as column chemistry, mobile phase composition, and gradient, on the separation efficiency of 21 commercially available FAHFA regioisomers without stated absolute configuration and 4 FAHFA enantiomers was assessed. The optimized SFC-MS method utilizes a chiral column based on a tris-(3-chloro-5-methylphenylcarbamate) derivative of amylose (Lux i-Amylose-3) and acetonitrile-methanol mobile phase modifier, enabling fast enantioseparation of most FAHFA racemic pairs in 5 min. However, the SFC separation of FAHFA regioisomers was less effective, limiting its applicability to complex biological samples. To address this, we propose an offline two-dimensional separation approach with reversed-phase liquid chromatography for isolating FAHFA regioisomers, followed by chiral SFC-MS analysis of fractions. The suitability of the method was demonstrated by characterizing the enantiomeric composition of FAHFA in white adipose tissue and rice samples. The chiral analysis revealed the presence of both R- and S-FAHFA isomers in the samples, with one enantiomer being predominant. SIGNIFICANCE: The developed approach represents a proof of concept for the use of SFC-MS with LC prefractionation for the characterization of FAHFA enantiomeric composition in complex biological samples, providing a valuable tool for future research on the biological roles of bioactive lipids in health and disease.

• Klíčová slova
• Chiral separation, FAHFA, Isomers, Lipids, Offline two-dimensional chromatography, Supercritical fluid chromatography,
• MeSH
• chromatografie kapalinová metody   MeSH
• estery * chemie   analýza   izolace a purifikace   MeSH
• hmotnostní spektrometrie * metody   MeSH
• hydroxykyseliny chemie   analýza   izolace a purifikace   MeSH
• mastné kyseliny * chemie   analýza   izolace a purifikace   MeSH
• myši MeSH
• stereoizomerie MeSH
• superkritická fluidní chromatografie * metody   MeSH
• zvířata MeSH
• Check Tag
• myši MeSH
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• estery * MeSH
• hydroxykyseliny MeSH
• mastné kyseliny * MeSH