Method Development and Validation in Food and Pharmaceutical Analysis

This reprint covers a wide range of topics including, but not limited to, new analytical and bioanalytical methods relevant to the separation, identification, and determination of substances in pharmaceutics, pharmacokinetics, nanobiotechnology, clinical chemistry, and related disciplines; methods for the identification of bioactive compounds in functional foods and medicinal plants; applications of chromatography and allied techniques in biomedical sciences

Neglected and Underutilized Plant Species in Horticultural and Ornamental Systems

This Special Issue contributes to filling knowledge gaps regarding NUS in horticultural and ornamental systems, as well as in landscapes, by collecting original research papers dealing with the relevance of NUS to the following topics: biodiversity and conservation; genetics and breeding; characterization, propagation, and ecophysiology; cultivation techniques and systems; landscape protection and restoration; product and process innovations; biochemistry and composition; and postharvest factors affecting their end-use quality

Aplicação das tecnologias de fluidos supercríticos e de líquidos pressurizados para a valorização dos rejeitos de cúrcuma : obtenção de compostos bioativos, custo de manufatura, equilíbrio de fases e encapsulamento dos extratos

Orientador: Maria Angela de Almeida Meireles PetenateTese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de AlimentosResumo: Além de ser uma perspectiva atual, a obtenção de compostos bioativos a partir de rejeitos agroindustriais é uma alternativa viável para o aproveitamento destes materiais, o que resulta na formação de produtos com características diferenciadas e alto valor agregado. No caso da cúrcuma (Curcuma longa L.), que possui vasta aplicação como corante natural, a quantidade de rejeito sólido gerado a partir dos processos de extração de óleos voláteis e curcuminóides (pigmentos amarelos) é elevada, e chega a atingir aproximadamente a quantidade de matéria-prima bruta utilizada para se realizar os procedimentos; por exemplo, para se obter óleo volátil por hidrodestilação, 98% de rejeito sólido é gerado para se obter da matéria-prima bruta apenas 2% de extrato. Esses resíduos possuem composição atrativa em termos de carboidratos que lhe conferem aplicação para a formulação de novos produtos, seja na forma de amido isolado, seja para produção de biofilmes ou açúcares simples e etanol a partir de hidrólise. Além de carboidratos, esses rejeitos possuem curcuminóides, que lhe conferem poder corante e efeitos antioxidantes. Diante disso, esta tese propõe alternativas sustentáveis para a valorização dos rejeitos de cúrcuma gerados a partir de processos que empregam fluidos supercríticos e líquidos pressurizados. Inicialmente foi investigado o cenário promissor da utilização de fontes não convencionais de amido para fins comerciais, além das tendências e perspectivas futuras para inclusão dos resíduos de cúrcuma como fonte complementar para o mercado de amidos. Posteriormente, foram investigadas duas alternativas para o aproveitamento dos rejeitos de cúrcuma, que consistem na realização de ensaios de hidrólise parcial com o uso de água pressurizada e na investigação do impacto das tecnologias de extração com dióxido de carbono supercrítico e etanol pressurizado na modificação física dos rejeitos de cúrcuma e nos subsequentes amidos isolados. A partir da reação de hidrólise foram estudados dois produtos, um extrato líquido e o rejeito sólido, ambos constituídos de curcuminóides e carboidratos. Não fugindo dessa questão do aproveitamento, o comportamento a altas pressões do rejeito parcialmente hidrolisado e dos óleos voláteis de cúrcuma foi estudado a partir do levantamento de dados de equilíbrio de fases empregando-se o método sintéticovisual sem retirada de amostra, cujo aparato experimental foi construído e validado nesta tese. Diante da baixa estabilidade e pobre absorção dos compostos bioativos da cúrcuma no organismo humano, foram realizados ensaios de encapsulação dos extratos de curcuminóides e óleos voláteis em polietilenoglicol com o intuito de oferecer um novo produto de maior estabilidade em termos de biocompostos com efeitos antioxidantesAbstract: In addition to being a current perspective, obtaining bioactive compounds from agroindustrial wastes is a viable alternative for the use of these materials, which results in the formation of products with differentiated characteristics and high added value. In the case of turmeric (Curcuma longa L.), which has a wide application as a natural dye, the amount of solid waste generated by the extraction of volatile oil and curcuminoids (yellow pigments) is elevated and reaches approximately the amount of the raw material used to carry out the procedures, i.e., to obtain volatile oil using hydrodistillation, 98% solid waste is generated to obtain only 2% crude extract from raw material. These residues have attractive composition in terms of carbohydrates that give it application for the formulation of new products, either as an isolated starch or for the production of biofilms or simple sugars and ethanol from hydrolysis. In addition to carbohydrates, these materials have curcuminoids, which attribute it colorant power and antioxidant effects. In this context, this thesis proposes sustainable alternatives for the valorization of the turmeric wastes generated from processes that use supercritical fluids and pressurized liquids. We initially investigated the promising scenario of the use of unconventional sources of starch for commercial purposes, as well as future trends and perspectives for inclusion of turmeric residues as a complementary source for the starch market. Afterwards, we investigated two alternatives aimed for the reuse of turmeric wastes, which consists of application of partial hydrolysis using pressurized hot water and the investigation of the impact generated by extraction technologies using supercritical carbon dioxide and pressurized liquid ethanol in the physical modification of turmeric wastes and the subsequently isolated starches. From the hydrolysis reaction, two products, i.e., a liquid extract and the solid waste, both consisting of curcuminoids and carbohydrates, were studied. High-pressure phase behavior of the turmeric partial hydrolyzed waste and volatile oils was studied through acquisition of phase equilibrium data using the synthetic-visual method without sample withdrawal, which experimental apparatus was constructed and validated in this thesis. In view of the low stability and poor absorption of turmeric bioactive compounds in the human body, encapsulation tests of curcuminoids ethanolic extract and volatile oils in polyethylene glycol were carried out in order to provide a new product with greater stability in terms of bioactives with antioxidant effectsDoutoradoEngenharia de AlimentosDoutora em Engenharia de AlimentosCAPE

Characteristics and properties of a polysaccharide isolated from Wolfiporia cocos as potential dietary supplement for IBS

IntroductionAs low FODMAP (Fermentable oligosaccharides, disaccharides, monosaccharides and polyols) diet therapy is recommended for most of Irritable Bowel Syndrome (IBS) patients, the consequent insufficient of dietary fibers (DFs) intake exert an adverse impact on intestinal health. It is necessary to find suitable DFs for IBS patients.MethodsThis study extracted a water-insoluble polysaccharide from Wolfiporia cocos (WIP) by alkali-extraction and acid-precipitation method. Its molecular weight was detected by high performance gel permeation chromatography (HPGPC) analysis. The structure of WIP was analyzed by Fourier transform infrared (FT-IR) spectrum, Nuclear Magnetic Resonance (NMR) spectra and X-ray diffraction (XRD). The properties related to stability, digestion, viscosity, osmotic activity, adsorption and fermentation were investigated, aimed to explore the feasibility of WIP as a new DF supplement for patients with IBS. In addition, 16S rRNA sequencing analysis was conducted to explore its effects on IBS-related gut microbiota.Results and DiscussionThe results showed that WIP had a single homogeneous composition and the molecular weight was 8.1 × 103 Da. WIP was indicated as a kind of pyranose form with β anomeric configuration and the main chain of WIP was 1,3-β-glucan with amorphous structure. In addition to good thermal stability, WIP also has low bioavailability and can reach the colon mostly without being digested. Moreover, the low viscosity and osmotic activity, the high water- swelling and water/oil-holding capacity, fructose adsorption capacity and poor fermentation performance of WIP demonstrated that it is suitable for IBS patients. It is worth noting that WIP regulates IBS associated gut microbiota effectively, such as the abundance of Lachnospiraceae and Prevotella. These findings provide a theoretical basis for the development of WIP as a dietary supplement for IBS patients with low FODMAP diet therapy.GRAPHICAL ABSTRAC

Functional Foods and Food Supplements

Recent technological advancements, socio-economic trends, and population lifestyle modifications throughout the world indicate the need for foods with increased health benefits. The clear relationship between the food that we eat and our well-being is widely recognized. Today, foods are not only intended to satisfy hunger and provide necessary nutrients: they can also confer additional health benefits, such as preventing nutrition-related diseases and improving physical and mental well-being. This book provides a comprehensive overview of developments in the field of functional foods and food supplements. Readers will discover new food matrices as innovative natural sources of bioactive compounds endowed with health-promoting properties. Studies on chemical, technological, and nutritional characteristics of healthy food ingredients, analytical methods for monitoring their quality, and innovative formulation strategies are included

Sensorial perception of astringency: oral mechanisms and current analysis methods

Understanding consumers’ food choices and the psychological processes involved in their preferences is crucial to promote more mindful eating regulation and guide food design. Fortifying foods minimizing the oral dryness, rough, and puckering associated with many functional ingredients has been attracting interest in understanding oral astringency over the years. A variety of studies have explored the sensorial mechanisms and the food properties determining astringency perception. The present review provides a deeper understanding of astringency, a general view of the oral mechanisms involved, and the exciting variety of the latest methods used to direct and indirectly quantify and simulate the astringency perception and the specific mechanisms involved.The research leading to these results has received funding from Nanotechnology-based functionalsolutions, funded by ERDF and CCDR-N, under the call Norte2020 (Ref. NORTE-01-0145-FEDER-000019)and the from FODIAC–Food for Diabetes and Cognition, funded by European Union, under the call MarieSkłodowsk-Curie Research and Innovation StaffExchange (Ref. H2020-MSCA-RISE-778388). This work was alsosupported by FCT with the reference project UID/EEA/04436/2019

Characterization of Volatile and Non-Volatile Compounds and Classification of Different Cultivars of Chinese \u3ci\u3eZiziphus jujuba\u3c/i\u3e Mill. Fruits

Jujube (Ziziphus jujuba Mill.) is a desirable fruit that is widely grown in China. Also, it has been used as an herbal medicine and a functional food simultaneously for a very long time. In this study, 15 cultivars of jujube that were collected from a same farm in Shanxi Province, China, were analyzed in terms of their non-volatile components, including reducing sugars, organic acids, fatty acids, amino acids, minerals and antioxidants, and volatile compounds, in an effort to investigate their nutritional values, and the similarity between the cultivars so as to classify the cultivars based on their chemical composition. The results showed that, in generally speaking, there were significant differences in the chemical compositions among the cultivars (p\u3c0.05). The content of glucose varied from 85.87 to 1004.95 mg/100g FW; malic acid and citric acid were main organic acids, of which the contents ranged from 120.15–508.67 mg/100g FW and 29.40–180.69 mg/100g FW, respectively. Jujube fruits contained a variety of polyunsaturated fatty acids, including linoleic acid, linolenic acid, eicosapentaenoic acid, arachidonic acid, and docosahexaenoic acid. In addition, the fruits were rich of lauric acid (967.20–4035.78 μg/kg DW), palmitic acid (685.68–1936.91 μg/kg DW), myristoleic acid (1718.96–5862.64 μg/kg DW), oleic acid (427.87–2864.98 μg/kg DW), linoleic acid (533.34–7330.05 μg/kg DW). Besides, iron (52.72–125.16 mg/kg DW), calcium (162.29–287.53 mg/kg DW) and magnesium (511.77–699.77 mg/kg DW) were also determined as the main minerals in the fruit. By using the hierarchical cluster analysis and principal component analysis, the 15 cultivars, based on the contents of reducing sugars, were classified into 6 groups, including group A (PZ and DB), group B (NP and LZ), group C (YZ, LB, XZ, HP, BJ and JB), group D (YL, JS, JD), group E (BZ) and group F (PB). Except the group E and group F, the other groups can be differientated from each other. Antioxidants including cAMP, ascorbic acid, triterpenes, and the total phenolic content, total flavonoid content, as well as the antioxidant capacity (i.e., FRAP, DPPH, ABTS, HRSA) were also analyzed in this study. According to the results, the content of cAMP was in a range of 66.33 to 2716.88 μg/100g FW; the content of ascorbic acid ranged from 317.9 to 679.6 mg/100g FW. In addition, jujube contained a low content of triterpenes (6.66 to 18.19 mg/100g FW). The total phenolic content was determined in a range from 330.74 to 571.44 mg gallic acid /100g FW, while the total flavonoids content varied from 43.14 to 154.09 mg rutin/100g FW. The range of antioxidant capacity such as DPPH, ABTS, FRAP and HRSA were determined to range from 0.603 to 1.842 mmol Trolox/100g FW, 2.276 to 2.786 mmol Trolox/100g FW, 1.228 to 3.823 mmol Trolox/100g FW, and 1.353 to 3.560 mmol Trolox/100g FW, respectively. All the 15 cultivars were classified into five clusters based on hierarchical cluster analysis. As a result, the cultivars of NP, JS, YZ were categorized in the same cluster, which contained relatively high contents of antioxidant components and strong antioxidant capacity. Solid phase micro extraction method (SPME) was used to extract the volatile compounds of jujube, which were further identified by GC–MS. The identified volatiles included aldehydes, alcohols, acids, ketones and esters. Among them, hexanal (276.5 to 1314 μg/100g FW), (E)-2-hexanal (145.1 to 1876 μg/100g FW), nonanal (188.2 to 1047 μg/100g FW), and n-decanoic acid (58.42 to 1268 μg/100g FW) were found to be the main volatile compounds in fresh jujube. Based on the contents of the volatile components, the jujube fruits were classified into five clusters, including cluster 1 (LB, HP, LZ, NP, JS, PZ, and YL), cluster 2 (BJ, DB), cluster 3 (PB, BZ, JD and XZ), cluster 4 (JB) and cluster 5 (YZ). Cluster 1, cluster 2 and cluster 3 were found to be crossed over together in the two-dimension plot, which means they could not be discriminated from each other based on contents of volatile compounds. However, the cluster 4 and cluster 5 could be separated very well from each other and from the other clusters. Moreover, two extraction methods, SDE and SPME, were compared in regards of their efficiency of extracting volatile compounds from the dried jujube fruits. (E)-2-Hexenal and hexanal were found to be the major aldehyde compounds in the SDE extract, while nonanal and benzaldehyde were major aldehyde compounds extracted by the SPME method

Synthesis and Characterization of Novel Polyester Scaffolds from Sugarcane Industry By-products for Use in Skin and Bone Tissue Engineering

The aim of this work was to synthesize non-toxic, biodegradable polyesters of aconitic acid, cinnamic acid and glycerol from by-products of the sugarcane industry as scaffolds for skin and bone tissue engineering. Utilizing the by-products, molasses and sugarcane bagasse, not only add value to the cane industry, but also paves path for synthesizing novel bio-based materials from the isolated specialty chemicals. Molasses contain an economically recoverable quantity of aconitic acid and its extraction was studied in detail as a part of this work. The yields of recovered aconitic acid varied from 25–69% depending on the extraction conditions. Under all the conditions, the purity values of extracted aconitic acid were higher than 99%. In the next step of the research, polyesters of aconitic acid, glycerol and cinnamic acid were synthesized. Different compositions of polyesters were characterized for their mechanical properties, porosity, mass loss in stromal medium, ability to support growth and proliferation of human adipose derived mesenchymal stem cells (hASC). Several biocompatibility tests such as mass loss over a period of time, alamar blue to analyze growth and viability of hASC on polyester scaffolds, picogreen for total DNA content synthesized indicated that these polyesters hold promising potential as tissue engineering scaffolds. The final step of this dissertation involved evaluating these polyesters as skin and bone tissue engineering scaffolds. For skin tissue engineering, especially wound repair, thin film polyester scaffolds laden with hASC were grown in stromal medium supplemented with basic fibroblast growth factor (bFGF). Based on the amount of collagen synthesized and DNA quantification data it was concluded that the polyesters can be used as scaffolds for wound repair by the addition of bFGF. The last step dealt with utilizing these as bone scaffolds where hASC were induced to undergo osteogenesis, and analyzed for mineralization and osteogenic target gene expression over a 21 days period. Based on calcium deposition results, and alkaline phosphatase (ALP) and osteocalcin (OCN) expression data, it was concluded that these scaffolds hold great potential for bone tissue engineering