MINISTRY OF EDUCATION AND TRAINING NONG LAM UNIVERSITY - HO CHI MINH CITY Faculty of Chemical Engineering and Food Technology MICROENCAPSULATION OF BIOACTIVE COMPOUND FROM GRAPE POMACE USING SPRAY DRYING A Thesis submitted in partial fulfilment of the requirements for admission to the degree of Bachelor of Engineering in Food Technology By Student: Le Mai Thao Nhi Supervisor: Assoc. Kha Chan Tuyen MSc. Nguyen Thi Thanh Thao Ho Chi Minh City, 2024 ACKNOWLEDGEMENT I would like to express my heartfelt gratitude to the teacher, friends, and family for the invaluable support and encouragement you provided while writing my graduation thesis and report. I want to especialy thank to the teachers in the Faculty of Chemical Engineering and Food Technology - Nong Lam University.
The teachers' engaging lectures, thorough knowledge of the subject matter, and sound guidance have all been very motivating for me to overcome obstacles and broaden my knowledge. I would like to express my deepest gratitude to Assoc. Kha Chan Tuyen and MSc. Nguyen Thi Thanh Thao for your valuable support and guidance throughout the process of completing my graduation thesis.
Your encouragement and constructive feedback have played an important role in shaping the quality and direction of my thesis. I appreciate the time and effort you spent reviewing my report and providing insightful suggestions, which helped me improve the overall quality of the project. Thanks to lab members for always helping me out. The discussions, difficult hours, and shared joys have made this journey more meaningful and memorable than ever.
Thank you sincerely! ABSTRACT The research entitled "Microencapsulation of bioactive compounds from grape pomace using spray drying" was conducted at the Faculty of Chemical Engineering and Food Technology, Nong Lam University, Ho Chi Minh City, from August 2023 to May 2024. The objective of the study was to determine the conditions affecting the microencapsulation of bioactive compounds in Red Cardinal grape pomace deep eutectic solvent extract using spray drying to obtain the maximum bioactive compound content contained in the spray-dried powder and high microencapsulation efficiency. Several factors were studied, including the type of DES solvent used to extract the bioactive compounds (Choline Chlorine:Glycerol: Citric Acid; Choline Chlorine:Lactic Acid), the core: wall material ratio (1: 5,1:6) and the type of wall material (maltodextrin, maltodextrin + isolated soy protein) to the content of TPC, PAC and the protective ability of the wall materials affect the spray drying microencapsulation process. The results show that the solvent Choline Chloride: Lactic Acid has high microencapsulation and powder recovery efficiency, so it was chosen to perform the extraction of bioactive compounds from grape pomace.
The core: wall material ratio of 1:6 led to the highest TPC and PAC microencapsulation efficiency (Š7.50 mg GAE/g DM, 44.17 mg CE/g DM, respectively). Moreover, the wall material combining maltodextrin (MD) and soy protein isolate (SPI) has enhanced the microencapsulation efficiency compared with maltodextrin. The maximum encapsulation efficiency, particularly for total phenolic compounds (TPC) and total proanthocyanidin content (PAC), was 73.79 mg GAE/g DM and 49.12 mg CE/g DM, respectively. i TABLE OF CONTENT ACKNOWLEDGEMENT sisessesssseosssnsssssccnsstssccntesavensossscoensonsecsnnvsscasanpnsnassessscnstoossssesses i ABSTRACT.
cscsssssssenssovessenassssnannssnasnsssaenesesetsnsvsssossnsvecsussvssnsowssenenensnssnsevenascnevesassueseovasts ii "FABLE OF ‘CONTEN D ssssssssvsnsenscnscesssessseossesessencnsvesssssuavnesoncanenvenssnveusssvenceresssesssceseses iii LIST OF ABBREVIATIONS .woscssscsssessensosssncsssvnesasnssorsnncsassanssescensenvensensscansensenssesonssse vi LIST OF TA BỊLE.-- << 5 <5 5< 5< << HH HH HH TH TH HH nung ngu nge vii EIS TE OE BIG Ung srercceanesessessgtbstlesst2xszagsEbxcsspsicgDoejgt2i3ssspsvsrvotee viii Chapter 1 DNTRODUCTION. các] SĂceiSeenaeiieskeekniesiaeiaskiaesasrasisdiszanseeii 1 Tels Ra f[DH4 ÍẾsssssesesseebeeseselensettdtlsbghesôslgsuggbuidBuslERiorto4g8Bsiifbag3ibsggchaxfidÐssordbsdlbgndào2S2189 sen 1 12M OF [HESEHDVaasireseetsoersossttionkb)gt100004g955013hbztyablosslitsbpubss9sbputbrclEp/8010000139) 2484 2 1. Scientific and practical sIø'n1ÍiCa'iCG.- ---- - 5 55 + 3111 9 nh nh ng nrư 2 1¿3.1; Setentifie significance) se ssscoissntosbtSESEIIOSEELS298S800-0i40388,502013/2383831318 means 2 13 22:.e†pniiTICBTIOEsxscaocsxsx6295696056150)4H2GHSG8G5GBSISGASVRSMIRGHLSESEGSRGOEEGBEISO.SSS8H01500300/2834 2 Chapter 2 LITERATURE REVIYYW.- SH HH HH HH HH HH ng ng 00006046. Qvefview Of øfaDe atid eF4D€ POMACE si 66c60 66g 1k0 0365413216610124638148138615 353884850634 3 2 |: l¿, OVERVIEW OF BTR Da sengnn tk n1 hĩ 5005966 61Xi0 i33 0103563 0x6188xi90138 8646014005518 L0E60318 488.2, OVERVIEW Of STADE POMACE can sns ng ng 011048158 3813003 G53N 5235E899853003548353680538.
Application of grape pomace (GP) in food system. Overview of bioactive chemicals found in grape pomace. Other bioactive compounds. Extraction methods and microencapsulation of grape extracts by spray drying ¬———.
10 21 Bod QWSFVIEW OF €STdDGÍivssseeiuenndeeiiiidasooasiosssi6348660000083503680600/1583160040338160370E 10 2. Technologies for the extraction of grape-pomace using Natural Deep Butectie Solverits: (Na DESS) sccsssessscsssocsmsxeasss H5E53i10SE233013GS. Overview of microencapsulation technoÏogy. Spray drying technology in encapsulating grape pomace microparticles .4, Factor which affect the efficiency Of SDE vss.
sssssssssnersesvssvsersvervsrecsenennss 15 Chapter 3 MATERIALS AND METHOD. Time and location of the experiments. Materials and MethodologByy. H1 tr re 18 oles eIESRC I AS sszszsyseosgo52gE2u8200u05.5đu80:0g563Eđice028dgQ8-SESI88/e°ti3t3S-giS.08ii2đ62g0cbSGifbEgic2ĐNrGi/20.1, Research material8 ssesssszearseeseotritiotistlgigpgat2g0ifxgiibZi6gi0583168i0:8118613352300230L533688E07830.28/8E 18 3212s EQUIPMECNUS wsccsscsensssessexscarerecaveneswertsesrsavereresemsienr ne mncmner eee 18 32.143 Git le Se 19 BD 2D, MOTO suy ng cere sees emer 010330001/E1EEDĐEAGSISEEEASSGHAR|SEEEIISSRESRGIGSEĐIBE4BNGOSIS24S810ã0288EL 19 3.
Raw material DTOGESSINHE PLOCeSS xeseccssesssecnevermcuanse name emremmmenaynaomaemnuneys 19 3. Deep eutectic solvent (DES) preparatIon. Extraction grape pomace pOwdet. Encapsulation of grape pomace extract and spray drying conditions.
Preparation of the emulsion and homogen1zaftion. Spray drying of encapsulation compound. Investigate the effect on the envelope of grape pomace extraction spray hla20tsvs1v2193011215L098i9ì1,111) 0. Experiment 1: Investigate the effect of solvent type on microencapsulation CLRICLET OS sescscennccerensapeormmarmnnanuneacnmi mir mnnemrerenene cee RIKEN ECR EET 24 3.
Experiment 2: Investigate the effect of core:wall material ratio on 00U409016:103111E10102022. Experiment 3: Investigate the effect of wall material microencapsulation CLFICTONCY 27277. Determination of total phenolic content (TPC). Determination of total proanthocyanin content (PAC).
Encapsulation Eliielehew (EE, '%) ssnsssscnsssssmnsensonsasavsssvovassnsanvsseseontassnanenass 27 3. Recovery yield of compounds (RY,%) .5: Powder f6GöXYSEÿV Field: (D6) can egennhnegggữ ngà ggggdgcaphšg8E15380518480811586093043105300g480.6, Data proceSsSin& MEMOS1T `“. cổ 28 8 2A, MOISTURE 'GGHIIGTEseeeeeenenebinby bionbssitbilitogtiptidbiitpiqdBUS/050/00G1048E3/E10530101201g8300:780020007Eg53. Scanning Electronic Microscopy (SEM) analyS1s.
snccesescennermrnavinaiersstommenircestaentesnennaurarenasmnueantnssy 28 Chapter 4 RESULT AND DISCUSSION. Experiment 1: Investigate the effect of solvent type on microencapsulation 2501019122223. 29 By) Ue POW G716 LH) k»sessssssebisbsbdgszdingioguszBinliqgszkdugdieisoirggsiribddglsogsndossderEtrôsursgtSZindaucug5528 29 4.-- ---- - -- 5< 3n ng ng tre 30 4.Partieal điiofppNGÌOĐWT-eeecsszaoeseebiisiddnniiucdinndtididgEdingi lich du DgEu150202dEg)La.Ea in TEmse 31 4. Experiment 2: Investigate the effect of core:wall material ratio on MICTOEN CAP SULA O fh P2777 ca cố ca co 33 4.-- - ¿2-55 555<<+<xc++es+eesex 34 4.
Experiment 3: Investigate the effect of wall material microencapsulation CML CLOH CY: eecsseseseveneseessereessnnesnseams 185653ĐSEERSSSSUSNGGESEGKLNSSIS934E383/9485ES85WELLSSSSSESGSSA.09S10960003838 36 43:1; Content of Compounds! (6) wrssessssscsusesenmvesse ere yesveemenmemneneuracmremesns 37 4. Recovery yield of compounds (%) .---- ------52< 2221222122222 2 rệt 39 Chapter 5 CONCLUSION AND RECOMMENDATION. RECOMIMENC ANON psn creceensces pases waseaucrastaasst S022 dGSietscigiRanrtGgsigs4sjiaigtGi2a-gg0 20 sal43 REFERENT CES vsissssssssssssssssosscencsnsuassccnnsancssssstnnestssavsseussvsssconssssesveavassantsansessssuesesessenses 44 APPEND UM ae ggggggg do 15046445) 43853454830588353438X3EKtuS33SSSN93SSSv4SSSSS44S63056355S5665658gEã.Gussg0 51 LIST OF ABBREVIATIONS ChCl1:Gly:CA Choline Clorine:Glycerol:Citric Acid ChCI:LUA Choline Clorine:Lactic Acid DES Deep Eutectic Solvents DM Dry matter g Gram mg Milligrams wiv Weight/volume w/w Weight/weight TPC Total polyphenol contents PAC Proanthocyanidins contents SPE Spay drying encapsulation MD Maltodextrin SPI Soy Protein Isolate C:W Core: Wall material vi LIST OF TABLE TaBIE 3-1? DES PrepaTratton ác ssesnsse sxoannsanasensnenssoarnnnennns.caasisnne sense 200 maosnaanteamerenunommanass 21 Table 3.1: Effect of DES solvent to color of GP powder after spray drying .2: Effect different type of wall materials to color of GP powder after spray vil LIST OF FIGURE Figure 2.1: Morphology of Microcapsules.1: Grape powder preparation procesS.2: Products during grape processing (a) grape pomace before processing; (b) remove branches and seeds; (c) grape pomace after dried; (d) grape pomace powder.3; ExtractiOi Pros xoscosesas-ccenesevenencescaccesesvseveesesueswenssancorevenan anesawanennernseeenens 22 Figure 3.4: Preparation for spray drying .-- ee 5< S1 eens cess ceeeeeeeeseneeeeeeeees 23 Figure 4.1: Effect of type DES on powder yIeÌd.- --- ----s-+++ss+scs+ecseeszrrrreeses 29 Figure 4. Effect of solvent type on TPC and PAC content microencapsulation CHCLEN CY: ALS SPRAY): CY 10 Bers iccnseeren sates erseemineaemnncitancamsita citer inn eamanateSrenaioes antares 31 Figure 4.
Scanning electron microsopy of grape pomace DES extract microencapsulated by spray drying (SD) using different solvents (a) ChCl:Gly:CA; (b) GHI LIA s06 pees bo S618 005600 GI2NGE-SDSLERRSHEDEISSEEENGLGRSIEREEEGRGHHENGMCEGGENGGGSEEESENGĐSIRIRNHSEAAS8E 32 Figure 4.: Microencapsulation of GP powder by spray drying (a) ChCL:LA; (b) ChCl: STC escent rece re cred SD ito ce eT INS to 33 Figure 4.5: Effect of core:wall material ratio on powder y1eld.9: Effect type of wall materials to recovery yield of compounds.10: Effect type of wall materials to recovery yield of compounds.11: Scanning electron microscopy (SEM) of GP powder microencapsulated by spray drying with different type of wall materials (a) MD; (b) MD+SPI.12: GP powder by using different type of wall materials after spray drying.42 Vili Chapter 1 INTRODUCTION 1. Rationale Nowadays, the consumption of foods containing several nutritional and health- promoting components is popular. Scientific research on polyphenols and their applications has recently garnered significant interest from the functional food, nutraceutical, and pharmaceutical industries due to their potential health benefits. Human diets contain polyphenols from fruits, vegetables, cereals, tea, essential oils, and their derived foods and beverages.
Among these, grapes are particularly noteworthy, not only as a food source but also for their bioactive compounds that can prevent numerous pathophysiological conditions, including cardiovascular diseases, neurodegenerative disorders, cancer, diabetes, and other ailments. Polyphenols are the most important phytochemicals in grapes, as they have numerous biological activities and health- promoting properties, including antioxidant, anti-inflammatory, antibacterial, and antiviral functions. The phenolic compounds mainly include anthocyanins, flavanols, flavonols, stilbenes (resveratrol), proanthocyanidins, and phenolic acids. The healthiest biomolecules found in grapes include proanthocyanidins, anthocyanins, various flavonoids, hydroxycinnamates, and stilbenes such as resveratrol.
These compounds are known for their antioxidant, antimicrobial, anti-cancer, and anti-inflammatory properties, and they also inhibit lipid peroxidation (Koyama, Kamigakiuchi et al. However, it is difficult to recover and preserve bioactive components from grapes. The resulting bioactive compounds are unstable, easily oxidized, and affected by heat, exposure to light, moisture contents, and pH. Microencapsulation has emerged as a vital technology to mitigate these challenges, enhancing the stability and extending the shelf life of these bioactive compounds without compromising their quality or activity.
Notably, the combination of spray drying and encapsulation technology has led to significant advancements in the extraction and preservation of grape-derived bioactive compounds. Spray drying, which operates at low temperatures and high pressures, effectively removes water while maintaining the stability of nutrients. This process reduces particle size and increases solubility and bioavailability, facilitating better absorption and utilization of grape nutrients by the body. The application of microencapsulation via spray drying not only improves the storage and transportation of these bioactive compounds but also enhances their accumulation in the body.
This innovative approach opens new avenues in the development of health-promoting food products and pharmaceuticals, leveraging the nutritional and therapeutic potential of grape-derived polyphenols. Based on all of these issues, the research project "Microencapsulation of bioactive compounds from grape pomace by using spray drying" was carried out. Aims of the study Overview of biologically active chemicals from grape by-products, using deep eutectic solvents during the extraction process to produce the highest concentration of biologically active compounds, and microencapsulating the extract using the spray drying method. Determine the appropriate type of wall material and the ratio between wall and core material to achieve the highest efficiency.
Scientific and practical significance 1. Scientific significance Determine the parameters of solvent type, ratio of core:wall materials, and type of wall material suitable for the spray drying process to extract bioactive compounds from grape pomace. The results of the project are the scientific basis for research related to spray drying of extracts from DES. Practical significance The results of the research are the basis for creating spray-dried powder from the extraction of bioactive compounds from grape pomace for applications such as preservatives and nutritional supplements.
Chapter 2 LITERATURE REVIEW 2. Overview of grape and grape pomace 2. Overview of grape Grapes have a lengthy history and are one of the most widely produced fruit crops worldwide. Grapes were revered during the ancient Greek and Roman civilizations for their use in winemaking.
Grapes are rich in vitamins (like vitamin C, vitamin K, and many B vitamins), carbohydrates, edible fiber and important minerals like potassium and manganese. Grape fruit and by products include a variety of bioactive compounds, including pigments, organic acids, and phenolic compounds (Tournour, Segundo et al. Grapes are now classified into three species: European grapes (Vitis vinifera), North American grapes (Vitis labrusca and Vitis rotundifolia), and French hybrids.