Characterization of cross-linked chitosan by ionic and covalent crosslinking agents as wall material of red ginger oleoresin microcapsules

Author(s):  
Jayanudin Jayanudin ◽  
Rochmadi Rochmadi ◽  
Fahrurrozi Moh. ◽  
Sang Kompiang Wirawan

The aim of this study was to determine the characterization of ionic and covalent interactions to form a crosslinking network with chitosan as a wall material of microcapsules. Red ginger oleoresin microcapsule was prepared by emulsion crosslinking method. Red ginger oleoresin was mixed and stirred with chitosan solution to form an emulsion, then added to corn oil and stirred again to form a second emulsion. Crosslinking agents of glutaraldehyde saturated toluene (GST) or sodium tripolyphosphate (TPP) solution was slowly added to the emulsion. When using a crosslinking agent of TPP solution was added glacial acetic acid to adjust pH. Red ginger oleoresin microcapsules were filtered and washed with petroleum ether followed by n-hexane and then dried in an oven. Microcapsules from chitosan that are cross-linked with GST produce higher yield and size of microcapsules compared to TPP. Whereas, the highest encapsulation efficiency produced from chitosan cross-linked with TPP was 91.63±0.02%. Meanwhile, the highest cumulative release was obtained from TPP cross-linked chitosan microcapsules of 63.71% and the lowest was 50.01% from chitosan microcapsules that cross-linked with GST. The conclusion of this study was the differences between ionic and covalent crosslinking agents produce different microcapsule characteristics. Microcapsules from chitosan cross-linked with GST generated more compact with a smoother surface than with TPP.

2017 ◽  
Vol 13 (2) ◽  
pp. 274 ◽  
Author(s):  
Jayanudin Jayanudin ◽  
Rochmadi Rochmadi ◽  
M. Kemal Renaldi ◽  
Pangihutan Pangihutan

The purpose of this study was to determine the effect of different coating materials on the efficiency of red ginger oleoresin encapsulation and characterization of microcapsule surface. The encapsulation process begins by dissolving chitosan with 1 % (v/v) acetic acid and dissolving sodium alginate using aquadest to be used as a coating material. Red ginger oleoresin alginate included in the solution was stirred. The mixture entered into the chitosan solution and added tween 80 was stirred using a homogenizer to emulsify. The emulsion that forms included in the <em>spray dryer</em> to be converted into a powder of microcapsules, and then analyzes the encapsulation efficiency and surface morphology of microcapsules using scanning electron microscopy (SEM). Differences in the coating material used were chitosan, mixture of chitosan-alginate and mixture of chitosan-alginate-sodium tripolyphosphate (STPP). Weight ratio of red ginger oleoresin and the coating material were 1: 1, 1: 2 and 1: 3. The research results obtained were the highest encapsulation efficiency obtained from the coating material of the chitosan-alginate-sodium tripolyphosphate (STPP) at a ratio of 1: 3, namely by 85 %.


2019 ◽  
Vol 17 (1) ◽  
pp. 228080001880991
Author(s):  
Jayanudin ◽  
Moh. Fahrurrozi ◽  
Sang Kompiang Wirawan ◽  
Rochmadi

Background: Encapsulation is one of the methods used to trap active ingredients in the wall material of microparticles. Aim: The aim of this study was to evaluate the encapsulation of red ginger oleoresin using an emulsion crosslinking method with chitosan as the wall material. Methods: Emulsions were formed of red ginger oleoresin with chitosan in concentrations of 1%, 2%, 3%, and 4% (w/v), respectively. The emulsions were then mixed with corn oil and stirred for one hour to obtain a second set of emulsions, and glutaraldehyde saturated toluene (GST) was added dropwise in quantities of 20, 10, 6.7, and 5 ml, respectively. This was followed by the addition of 2 ml of 25% glutaraldehyde and the emulsions were stirred for two hours. The resulting microcapsules were washed with petroleum ether followed by hexane and then dried in an oven at 70oC. Results: The emulsion crosslinking method used to trap the red ginger oleoresin in chitosan produced microcapsules of good spherical geometry with the mean diameter ranging from 75.61 ± 11.8 µm to 178.65 ± 40.7 µm. The highest yield was 98.93% and encapsulation efficiency was 83.1%. Thermogravimetric and differential thermal analysis showed that the melting point was at a temperature between 120 and 130oC. Conclusion: Chitosan concentration has little effect on encapsulation yield, whereas the amount of GST tends to strengthen the crosslinking bonds of chitosan and reduces the mean diameter of microspheres.


Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 742 ◽  
Author(s):  
Maiz-Fernández ◽  
Pérez-Álvarez ◽  
Ruiz-Rubio ◽  
Pérez González ◽  
Sáez-Martínez ◽  
...  

Stable hyaluronic acid nanogels were obtained following the water-in-oil microemulsion method by covalent crosslinking with three biocompatible crosslinking agents: Divinyl sulfone, 1,4-butanediol diglycidyl ether (BDDE), and poly(ethylene glycol) bis(amine). All nanoparticles showed a pH-sensitive swelling behavior, according to the pKa value of hyaluronic acid, as a consequence of the ionization of the carboxylic moieties, as it was corroborated by zeta potential measurements. QELS studies were carried out to study the influence of the chemical structure of the crosslinking agents on the particle size of the obtained nanogels. In addition, the effect of the molecular weight of the biopolymer and the degree of crosslinking on the nanogels dimensions was also evaluated for BDDE crosslinked nanoparticles, which showed the highest pH-responsive response.


2021 ◽  
Vol 15 (1) ◽  
pp. 40-46
Author(s):  
Jayanudin Jayanudin ◽  
◽  
Mohammad Fahrurrozi ◽  
Sang Kompiang Wirawan ◽  
Rochmadi Rochmadi ◽  
...  

In this study, chitosan-based carrier of red ginger oleoresin was prepared using the emulsion cross-linking technique with sodium tripolyphosphate (TPP) as a cross-linking agent. The effect of chitosan and TPP concentration, as well as pH on the encapsulation efficiency, particle size and characterization of chitosan microcapsule was determined. The antioxidant activity of microcapsules was analyzed. Chitosan microcapsules containing red ginger oleoresin were produced although with non-smooth surfaces.


2021 ◽  
Author(s):  
Aysegul Uzuner Demir ◽  
Fatih Arican ◽  
Aykut Sancakli ◽  
Ezgi Ismar

Abstract The leather industry, due to its way of using chemicals during treatment and releasing them back to the environment makes it one of the hazardous sectors. It is not only releasing the chemicals also during the process precious biomass such as collagen and keratin discarded as waste. In this study, bovine hair which occurs during the treatments of the bovine leather process is supplied as waste and converted to superabsorbent hydrogel via grafting of keratin with monomers (Acrylic Acid (AA), Acrylamide (AAm)) in the presence of N, N'-methylene bisacrylamide (NMBA) used as a crosslinking agent and ammonium persulfate (APS) as an initiator. Keratin is selected to enhance the biocompatibility of the hydrogel. Thus, different keratin/monomer ratios, crosslinking agents, and initiator amounts were accepted as variables, and reaction conditions were optimized to achieve the highest swelling capacity. Synthesized hydrogels were chemically, morphologically, and thermally characterized via Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), differential scanning calorimeter (DSC), and thermal gravimetric analyzer (TGA). FTIR, DSC, and TGA results confirmed the grafted structure. The maximum swelling ratio was recorded at pH 9, at the end of 48 hours as 1791%. Sponge-like hydrogels were successfully obtained, and waste keratin is successfully valorized by means of hydrogels which can be used in high-value-added areas.


2018 ◽  
Vol 14 (2) ◽  
pp. 178
Author(s):  
Jayanudin Jayanudin ◽  
Rochmadi Rochmadi ◽  
Moh. Fahrurrozi ◽  
Sang Kompiang Wirawan

<p>Tujuan penelitian ini adalah menentukan persamaan empiris dari bilangan tak berdimensi untuk memprediksikan ukuran mikrokapsul oleoresin jahe merah. Metode enkapsulasi yang digunakan adalah <em>crosslink</em> emulsi dengan kitosan sebagai penyalut dan <em>glutaraldehyde saturated toluene</em> (GST) sebagai agen <em>crosslink</em>. Oleoresin jahe merah dan kitosan dengan konsentrasi 1, 2, 3 dan 4% (w/v) diaduk dengan kecepatan 10.000 rpm untuk membentuk emulsi, kemudian dimasukan dalam minyak jagung dan diaduk kembali untuk membentuk emulsi kedua. Sebanyak 10 mL <em>glutaraldehyde saturated toluene</em> (GST) sebagai agen <em>crosslink</em> ditambahkan secara bertahap. Setelah itu, ditambahkan larutan glutaraldehida 25% dan terus diaduk selama 2 jam. Mikrokapsul dipisahkan dan dicuci dengan petroleum eter dan heksan, kemudian dikeringkan dalam oven dengan suhu 70 °C. Dengan cara yang sama digunakan untuk membuat mikrokapsul pada kecepatan pengadukan 5.000, 8.000 dan 15.000 rpm. Ukuran diameter mikrokapsul dianalisis menggunakan mikroskop digital. Persamaan empiris dari bilangan tak berdimensi Reynolds (<em>Re</em>) dan Ohnesorge (<em>Oh</em>) dibuat untuk memprediksikan diameter mikrokapsul. Data dari variabel perubahan konsentrasi kitosan dan kecepatan pengadukan dapat menghasilkan persamaan empiris dari bilangan Reynolds (<em>Re</em>) dan Ohnesorge (<em>Oh</em>). Konstanta yang dihasilkan adalah  = 422,06,  = 0,37 dan  = -0,18. Berdasarkan perbandingan antara data diameter penelitian dan hasil perhitungan didapat % kesalahan sebesar 8,05% untuk pengaruh konsentrasi kitosan dan 7,52% untuk pengaruh kecepatan pengadukan.</p><p><strong>A Simple Empirical Equation for Predicting Particle Size from Encapsulation of Red Ginger Oleoresin. </strong>This study aims to determine the empirical equations of the dimensionless number to predict the diameter size of red ginger oleoresin microcapsules. The encapsulation method used is crosslinking emulsion with chitosan as coating and glutaraldehyde saturated toluene (GST) as a crosslinking agent. Red ginger oleoresin and chitosan with concentrations of 1, 2, 3 and 4% (w/v) were stirred at 10,000 rpm to form emulsions, and then added to the corn oil and stirred again to form a second emulsion. The 10 mL of glutaraldehyde saturated toluene (GST) as a crosslinking agent was added gradually. After that, a 25% glutaraldehyde solution was added and stirred for 2 hour. Microcapsules were separated and washed with petroleum ether and hexane, then dried in an oven at a temperature 70 °C. The same step, the microcapsules were made at stirring speed of 5,000; 8,000; and 15,000 rpm. The size of the microcapsule diameter was analyzed using a digital microscope. The empirical equations of the dimensionless numbers Reynolds (<em>Re</em>) and Ohnesorge (<em>Oh</em>) are made to predict the microcapsule diameter. The data from the chitosan concentration change and stirring speeds could produce the empirical equations of the Reynolds and Ohnesorge numbers. The resulting constants were  = 422.06,  = 0.37 dan  = -0.18. By comparing the data diameter of the research and calculation results obtained % error of 8.05% for the influence of chitosan concentration and 7.52% for the effect of stirring speed.</p><div> </div>


2013 ◽  
Vol 821-822 ◽  
pp. 1051-1054 ◽  
Author(s):  
Ke Xi Zhang ◽  
Zhu Zheng ◽  
Xiao Feng Zhang ◽  
Xiao Hong Wang

In this article,cassava starch was cross-linked by crosslinking agent sodium tripolyphosphate in the microwave oven. The effect of microwave time on the cross-linking degree and morphology of cross-linked starch were investigated. The results show that with the increase of microwave processing time, the degree of crosslinking of starch increases.Phosphate ester group is formed on the starch molecular chains and the structure of cross-linked starch becomes amorphous by microwave irradiation .


2013 ◽  
Vol 14 (3) ◽  
Author(s):  
Eriawan Rismana ◽  
Susi Kusumaningrum ◽  
Olivia Bunga P ◽  
Idah Rosidah ◽  
Marhamah Marhamah

The chitosan – Garcinia Mangostana extract nanoparticles has been prepared by ionic gelation reaction by mixture 0.2 % chitosan solution in acetic acid with Garcinia Mangostana extract and it’s continued by reaction process with 0.1 % sodium tripolyphosphate. The particle size of material was determined by Particle Size Analyzer (PSA) that it showed in the range of 200 – 500 nm. The color, pH, water, α- mangostin, mercury, arsenic, cadmium, lead, totally microbe aerobic, totally mold and yeast, and solvent residue contents of nanoparticles were also examined by many methods that these resulted are yellow, 4.50 – 5.50, 89 – 90 %, 1.05 %, < 0.005 ppm, < 0.01 ppm, < 0.01 ppm, < 0.05 ppm, < 10 CFU/g, < 10 CFU/g and not detected, respectively. The other characterization was also observed that it’sincluded stability andTLC chromatogram. A mixture of nanoparticles with cosmetics bases was showed that it’s increased stability, homogeneity and easy to formed.


2021 ◽  
Author(s):  
Madhvi Garg ◽  
Navneet Bhullar ◽  
Bharat Bajaj ◽  
Dhiraj Sud

The present manuscript reports the ultrasound radiation induced synthesis of grafted chitosan hydrogels (CAAT and CAAG) using terephthalaldehyde/glutaraldehyde as crosslinking agents and its application for removal of synthetic dyes from...


Polymers ◽  
2021 ◽  
Vol 13 (5) ◽  
pp. 677
Author(s):  
Sara A. Abosabaa ◽  
Aliaa N. ElMeshad ◽  
Mona G. Arafa

The objective of the present research is to propose chitosan as a nanocarrier for caffeine—a commonly used drug in combating cellulite. Being a hydrophilic drug, caffeine suffers from insufficient topical penetration upon application on the skin. Chitosan nanoparticles loaded with caffeine were prepared via the ionic gelation technique and optimized according to a Box–Behnken design. The effect of (A) chitosan concentration, (B) chitosan solution pH, and (C) chitosan to sodium tripolyphosphate mass ratio on (Y1) entrapment efficiency percent, (Y2) particle size, (Y3) polydispersity index, and (Y4) zeta potential were studied. Subsequently, the desired constraints on responses were applied, and validation of the optimization procedure was confirmed by the parameters exhibited by the optimal formulation. A caffeine entrapment efficiency percent of 17.25 ± 1.48%, a particle size of 173.03 ± 4.32 nm, a polydispersity index of 0.278 ± 0.01, and a surface charge of 41.7 ± 3.0 mV were attained. Microscopical evaluation using transmission electron microscope revealed a typical spherical nature of the nanoparticles arranged in a network with a further confirmation of the formation of particles in the nano range. The results proved the successful implementation of the Box–Behnken design for optimization of chitosan-based nanoparticles in the field of advanced polymeric systems for pharmaceutical and cosmeceutical applications.


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