Source: UNIVERSITY OF ILLINOIS submitted to
MICROENCAPSULATION TECHNOLOGY USING A THREE FLUID NOZZLE AND SPRAY DRYING
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
COMPLETE
Funding Source
Reporting Frequency
Annual
Accession No.
1013950
Grant No.
(N/A)
Cumulative Award Amt.
(N/A)
Proposal No.
(N/A)
Multistate No.
(N/A)
Project Start Date
Oct 1, 2017
Project End Date
Sep 30, 2022
Grant Year
(N/A)
Program Code
[(N/A)]- (N/A)
Recipient Organization
UNIVERSITY OF ILLINOIS
2001 S. Lincoln Ave.
URBANA,IL 61801
Performing Department
Food Science & Human Nutrition
Non Technical Summary
Microencapsulation is defined as a technology of packaging solids, liquids, or gaseous materials in miniature, sealed capsules that can release their contents at controlled rates under specific conditions. Encapsulation technology in food processing consists of coating minute particles of ingredients (e.g., acidulants, fats, and flavors), as well as whole ingredients (e.g., raisins, nuts, and confectionery products), by microencapsulation and macrocoating techniques, respectively. Microcapsules offer the food processor a mean to protect sensitive food components, ensure against nutritional loss, utilize otherwise sensitive ingredients, incorporate unusual or time release mechanisms into the formulation, mask or preserve flavors and aromas, and transform liquids into solid ingredients that are easy to handle.Food ingredients, enzymes, cells, or other materialscan be encapsulated by many different techniques including physical methods (e.g., spray drying and extrusion), chemical methods (e.g., interfacial polymerization), and physicochemical methods (e.g., coacervation). Among those techniques, spray drying is the most common and economical technique to produce microencapsulated food materials. Liquids are atomized by centrifugal atomizer or nozzle and immediately dried by hot air flowing in the chamber. The main advantage of the spray drying is the ability to handle labile materials because of the short contact time in the dryer. Various polymer systems such as alginate, carrageenan, protein, and starch have been used to encapsulate target materials using spray drying. Protein and carbohydrate are the most commonly used as wall materials in microencapsulation due to their good encapsulation properties.A conventional route to form a core-shell structure requires mixing of two immiscible phases in order to generate an emulsion, which is generally an energy intensive process. The emulsion is pumped through an inner channel and transformed into mist by a compressed gas flowing through the outer channel. In addition to the need for the step to create an emulsion, it is difficult to encapsulate two miscible materials in a core-shell structure using a two-fluid nozzle. The focus of this proposed project is to encapsulate various target materials in core-shell structures using a three-fluid nozzle.A three-fluid nozzle has three fluid channels; a center channel for liquid 1 (target material), a middle channel for liquid 2 (wall material), and a outer channel for compressed gas. One of the notable advantages of using a three-fluid nozzle is that the core-shell structure can be formed with a one-step process without requiring any pre-treatments such as pre-mixing or pre-homogenization. Also, it is possible to form a core-shell structure with two miscible materials.
Animal Health Component
30%
Research Effort Categories
Basic
30%
Applied
30%
Developmental
40%
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
5015010202050%
5025010202050%
Goals / Objectives
Our long term goal is to provide a novel technique for a microencapsulation that can be applied to a wide range of applications. We hypothesize that the adaptation of a three-fluid nozzle to spray drying will enable the formation of core-shell structures without energy intensive additional steps. For this long term goal, three specific aims were developed.The specific aims include:1. Revise the design of three-fluid nozzle to improve the formation of core-shell structuresThe working hypothesis for Aim 1 is that the design of the three fluid nozzle is a critical factor and the relative length of the center, middle and outer channels of the three-fluid nozzle will be the main factor to form and control the core-shell structure.2. Identify the additional factors to control core-shell structure of encapsulated particles.The working hypothesis for Aim 2 is that there are inter-related factors in spray drying to control the core-shell structure of microcapsules. The inter-related factors may include the viscosity, surface tension, absolute flow rate, and relative flow rate of the two liquids.3. Apply the three fluid nozzle to encapsulate various target materials.The working hypothesis for Aim 3 is that the spray drying using a three-fluid nozzle can be applied to encapsulate a wide range of target materials including solid-lipid carriers, hygroscopic materials in core-shell structures.
Project Methods
Objective 1. Revise the design of three-fluid nozzle to improve the formation of core-shell structure. The current design of the three-fluid nozzle has the same length for the center, middle and outer channels.This design is simple but provides limited coverage of the core material due to the same discharge points for both core and wall materials. The design will be revised to implement different lengths for each channel so the core material will be encapsulated by the wall material completely. The modification will be made at the Electrical & Computer Engineering machine shop at the University of Illinois, Urbana-Champaign.The material used for this aim will be whey protein isolate (WPI) as a wall material and anhydrous milk fat (AMF) as a core material. The spray dried microcapsules using the revised nozzle design will be analyzed for morphology and surface oil content. The design of the three-fluid nozzle will be revised to improve the coverage of the core material. The spray drying will be conducted with inlet temperature of 170 degrees C and outlet temperature of 90 degrees C.Objective 2. Identify the additional factors to control core-shell structure of encapsulated particles.There are many factors affecting a spray drying process. In this proposed study, viscosity, total flow rate of liquid 1 and 2, and flow rate ratio between liquid 1 and 2 will be controlled. The viscosity of liquid 1 and 2 will be adjusted by varying solid concentration and feed temperature. The materials to be used for this aim is the same as the aim 1; WPI and AMF. To assess the effect of the factors on the microcapsule formation, morphology and surface oil content will be analyzed.Objective 3. Apply the three-fluid nozzle to encapsulate various target materials.Based on the nozzle design fromaim 1 and the factors fromaim 2, the spray drying with a three-fluid nozzle will be applied for various core materials.The first type of core materials will be a solid lipid particle encapsulated using WPI and AMF. Fat soluble bioactive compounds such as oregano essential oil or tributyrin will be dispersed in AMF and encapsulated using the three-fluid nozzle. The particle morphology, encapsulation efficiency and release profile of the bioactive compounds will be analyzed. The morphology will be assessed using a Scanning Electron Microscopy (SEM). The encapsulation efficiency will be analyzed by quantification of the core materials in microcapsules using a high-performance liquid chromatography (HPLC) and a gas chromatography (GC) and comparing it with the amount initially added to the microcapsule. The encapsulation efficiency will be calculated by the following equation:Encapsulation Efficiency (%) = (Amount of core detected in microcapsule / Amount of core added) x 100The release profile of the bioactive compound will be analyzed by measuring the concentration of the target bioactive compound in a solvent (for example water) after dispersing the microcapsules in the solvent. The concentration of the bioactive compound will be measured over period of time until a concentration equilibrium is achieved.To investigate the release of bioactive compounds in digestive system, a static in-vitro digestive model will be used. The in-vitro model will be composed of three phases: oral, stomach, and small intestinal phases. The microcapsules will be placed in each phase in sequence and incubated at 37 degrees C. The release of the bioactive compound from the microcapsules will be analyzed using a HPLC and a GC.The second type of core materials will be a hygroscopic material such as oligosaccharides. Hygroscopic materials are extremely difficult to spray dry due to their low glass transition temperature (Tg). When Tg is low, the material tends to stick on various surfaces during the spray drying process and results in very low yields. Microencapsulation may be able to provide a thin layer of coating with high Tg to prevent the stickiness issue occurring during spray drying as well as storage. Oligosaccharides will be used as a hygroscopic core material and maltodextrin will be used as a wall material. The yield, encapsulation efficiency, morphology, and storage stability will be assessed. The yield is the measurement of ration between the collected spray dried material and total material fed into the spray dryer. The encapsulation efficiency will be calculated using the equation above and morphology will be assess using the same SEM as explained above. The encapsulated hygroscopic material will be sealed in airtight containers and stored at room temperature and at 40 degrees C for an extended period (at least three months). The glass transition temperature, moisture content, degree of aggregation will be measured to evaluate the storage stability.

Progress 10/01/19 to 09/30/20

Outputs
Target Audience:This project is targeting the scientific community and product developers who are interested in improving microencapsulationtechnology. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?A graduate student have been trained during this project year. The student hasbeen trained to develop new nozzle design and a spray drying with the various nozzle configurations. The student also has been trained for various analytical techniques. How have the results been disseminated to communities of interest?The results have been shared with several companies. However, the experiments have not been completed and more results will be disseminated to thescientfic community next year. What do you plan to do during the next reporting period to accomplish the goals?The entire trials in the experimental design will be completed. The clear impact of pectin concentration on the encapsulation efficiency, particle properties, as well as the impact of the properties of encapsulated oil will be assessed.

Impacts
What was accomplished under these goals? Prototype three fluid nozzle was developed. The inner nozzle channel has been modified to allow variation of the contact time between fluid 1 and fluid 2. Maltodextrin DE-10 (Ingredion, Westchester, Illinois) and sugar beet pectin (CP Kelco, Atlanta, Georgia) were selected as the wall material for the encapsulation by spray drying affected by the feed material properties. Wall material solutions were prepared as the formulation in the range of 10-20% of Maltodextrin and 0.5-4% of pectin.After dissolving pectin and maltodextrin into the DI water completely, the solution was kept stirring overnight for the following measurements or experiments. Soybean oil (ALDI, Batavia, Illinois) was selected as the model core material, and there was no treatment for the soybean oil before spray drying. The density of soybean oil is 0.9 g/mL. The rheological properties of wall material solutions were measured using ARES-G2 rheometer (TA Instruments, New Castle, Delaware). For each formulation of the wall material, experiments were conducted in triplicateusing approximately 30 mL of sample for each measurement. The measurements were performed at 25 degrees C from 0.1 to 100 1/s of shear rates. The geometry used was DIN concentric cylinder (bob diameter of 27.7 mm and cup diameter of 30 mm). The resulting curve was fit with Power-Law fluid where: K is the flow consistency index (SI units Pa sn); is the shear rate or the velocity gradient perpendicular to the plane of shear (SI unit s-1); is the flow behavior index (dimensionless). The concentration of pectin and maltodextrin had significant impact on the rheological properties of the wall matrial solutions. As concentration of wall materials, especially pectin, increased, the consistency index increased and flow behavior index decreased. Soybean oil was encapsulated in the maltodextrin-pectin wall and the encapsulation efficiency was higher than 80% even without prehomoginization, which is a promising result.

Publications


    Progress 10/01/18 to 09/30/19

    Outputs
    Target Audience:This project is targeting the scientific community and product developers who are interested in improving microencapsulation technology. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?A graduate student have been trained during the project year. The student have been trained to develop new nozzle design and a spray drying with the various types of nozzles. The student also has been trained for various analytical techniques. How have the results been disseminated to communities of interest?The results from this project year have been reported at the Institute of Food Technologists Annual Meeting (IFT 2019). The previous study was published in a peer reviewed journal. What do you plan to do during the next reporting period to accomplish the goals?The study on nozzle design will be carried out more and the effect of nozzle design on the encapsulation performance will be analyzed.

    Impacts
    What was accomplished under these goals? During this period, the continuing nozzle design was carried out. The design of three-fluid nozzle (3FN) was modified to explore the effect of interaction between the materials in inner (core material) and outer (wall material) channels. Maltodextrin (DE10) and oligosaccharide were used for this study. Samples were spray-dried using either a two-fluid nozzle (2FN) or two types of 3FN (long and short inner nozzle tips). These inner nozzles were modified from the original version of nozzle tips. Oligosaccharide (OS) was used as a low molecular weight material and maltodextrin DE10 (MD10) as a drying aid. For 3FN, OS was fed through the inner channel and MD10 through the outer channel, separately. For 2FN, FOS and MD10 were premixed and spray dried. Inlet and outlet temperatures were 160°C and 90°C, respectively. Spray drying with 45% OS in the feed resulted in higher yields (54-64%) than 70% OS in the feed or OS without MD10. The stability of the powder was determined by the glass transition temperature (Tg) for thermal stability and by equilibrium absorption isotherms for water sorption stability. Two separate Tgs in the ranges of 40-45°C and 60-65°C were observed in the samples with the 3FNs, suggesting the presence of two isolated materials in the powder. The equilibrium sorption isotherms showed an improved water sorption stability for the samples dried with the 3FNs compared to spray-dried OS powder. When the 3FNs were used, the stability of powder was improved while reducing the amount of drying aids and eliminating a mixing step before spray drying.

    Publications

    • Type: Conference Papers and Presentations Status: Published Year Published: 2019 Citation: Luis G. Luna-Alanis and Youngsoo Lee. 2019. Spray drying of fructooligosaccharides (FOS) using a three-fluid nozzle. Institute of Food Technologists 2019, New Orleans.
    • Type: Journal Articles Status: Published Year Published: 2019 Citation: Jingwen Cai and Youngsoo Lee. 2019. Controlling sodium release using maltodextrin and octenyl-succinic-anhydride-modified starch with two types of spray-dryer nozzles. J. Food Proc. Eng. E13238.


    Progress 10/01/17 to 09/30/18

    Outputs
    Target Audience:This project is targeting the scientific community and product developers who are interested in improving microencapsulation technology. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?Two graduate students have been trained during the project year. The students have been trained to develop microencapsulation processes using a spray drying with various types of nozzles. The student also has been trained for various analytical techniques including physical, chemical, and sensory analyses. How have the results been disseminated to communities of interest?The results from this project year have been reported at the Conference of Food Engineering (CoFE) and a peer-reviewed articles is being prepared. What do you plan to do during the next reporting period to accomplish the goals?The study on nozzle design will be carried out more and the effect of nozzle design on the encapsulation performance will be analyzed.

    Impacts
    What was accomplished under these goals? During this period, sodium was encapsulated in two types of matrices using a spray drying withtwo- or three-fluid nozzles. Controlling release of sodium during oral processing of food is a promising way to achieve sodium reduction in food products. Microencapsulation is a potential technique to control the sodium release. The objective of this study was to develop sodium chloride-loaded microcapsules and to characterize the sodium release of those microcapsules. Maltodextrin (DE10) and octenyl succinic anhydride (OSA) modified starch were evaluated as carriers to create microcapsules using spray drying with a 2-fluid and 3-fluid nozzle. For the 2-fluid nozzle, the carrier solution (5 or 10% w/w) and NaCl solution (25% w/w) were mixed before spray drying. For the 3-fluid nozzle, the carrier solution and NaCl solution flowed separately through two different channels without mixing for the spray drying. The morphology of microcapsules was observed by Scanning Electron Microscope (SEM). The SEM images showed most sodium was encapsulated into the carriers successfully. Microcapsules made with OSA modified starch had more smooth, round, and uniform spherical shape than with the maltodextrin samples. The sodium release was measured in the form of total dissolved solids using a conductivity probe. Increasing the concentration of OSA modified starch significantly decreased Rmax (maximum sodium release rate), C50 (sodium concentration at 50s) and C150 (sodium concentration at 150s) and the same trend was observed for the maltodextrin. Generally, the samples spray dried with a 2-fluid nozzle released sodium faster than the samples with a 3-fluid nozzle. This study indicated the delivery of sodium could be altered by using various type and concentration of carriers as well as the type of spray dry nozzles, which may provide strategies to reduce sodium content in foods, especially salty snack foods.

    Publications

    • Type: Conference Papers and Presentations Status: Accepted Year Published: 2017 Citation: Jingwen Cai and Youngsoo Lee. 2018. Controlling sodium release using maltodextrin and octenyl succinic anhydride (OSA) modified starch with two types of spray dryer nozzles, CoFE 2018, Minneapolis.