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Membrane Technology Application for Fractionation Process to Obtain High Quality Glucosamine Rokhati, Nur; Istirokhatun, Titik; Hamada, Nur ?Aini; Apriyanti, Dwi Titik
Reaktor Volume 20 No.2 June 2020
Publisher : Dept. of Chemical Engineering, Diponegoro University

Glucosamine, monosaccharide from chitosan obtained from the chitin deacetylation process, has been used widely in various fields such as nutrition, pharmacy, and cosmetics. Glucosamine can be obtained from the hydrolysis of chitosan. Enzymatic hydrolysis provides the advantage of mild reaction conditions, environmentally friendly, and high yield. But until now, the separation of glucosamine from the chitosan hydrolysis fraction has been an obstacle. Ultrafiltration membranes offer an efficient filtration process because they do not require additional chemicals. The performance of ultrafiltration membranes was analyzed from the fractionation process of chitosan hydrolysis. The PES membranes in 10, 25, and 50 kDa were used to filter hydrolyzed Low Molecular Weight Chitosan (LMWC) in varied concentrations. The experiment was carried out in crossflow membrane module for flat sheet at room temperature in 1 bar. The permeate flux during filtration decreased rapidly at the initial and gradually over time because of fouling and concentration polarization. The more concentrated hydrolyzed LMWC solution resulted higher percentage of rejection up to almost 20% at the same membrane MWCO while higher MWCO resulted lower rejection percentage for the same hydrolyzed LMWC concentration. The FTIR spectrum of the used membranes of all types had absorption bands of glucosamine which proved that the fractionation process occurred. The time retention in HPLC chromatograms of glucosamine produced were similar with standard glucosamine. Thus, ultrafiltration could be applied for hydrolyzed LMWC fractionation process.Keywords: fractionation; glucosamine; LMWC; MWCO; ultrafiltration

Application of Glyoxal Acrylamide Modified Κ-Carrageenan as A Superabsorbent Polymer in Drug Delivery System Aji Prasetyaningrum; Al Farrel A. Raemas; Nur Rokhati; Bakti Jos
Reaktor Volume 20 No.3 September 2020
Publisher : Dept. of Chemical Engineering, Diponegoro University

The hydrogel is superabsorbent polymers (SAP) that are biodegradable and can be obtained from polysaccharides, lipids, and proteins. Polysaccharides include cellulose, starch and their derivatives, seaweed extracts such as carrageenan, alginate, pectin, and chitosan. Carrageenan is the result of the extraction of red seaweed sap with an alkaline solution. The main objective of this study was to simultaneously increase the strength and properties of κ-carrageenan SAP film with the addition of glyoxal and acrylamide as crosslinkers. The addition of acrylamide (variated from 1 to 7 % b/v) into the k-Carrageenan based SAP hydrogel compound and the presence of glyoxal as crosslink agent (variated from 0 to 1,0 % v/v). The physical properties of the SAP films were analyze using swelling degree and tensile strength. The structural and morphological properties of composite films were analyzed using Fourier Transform Infrared (FTIR) and Scanning Electron Microscopy (SEM). In addition, the effect of pHs on the releasing drug Poly(vinylpyrrolidone)-Iodine was investigated. This research shows that the addition of acrylamide and glyoxal can improve the physical properties of the modified κ-carrageenan film. Characterization using SEM shows that the addition of glyoxal causes the formation of tissue fibers in SAP. FTIR spectra indicated the formation of cross bonds in modified SAP film at 3294.42 cm-1 (carboxylic acid). The treatment under alkaline conditions will increase drug release ability.Keywords: κ-carrageenan; hydrogels; acrylamide; glyoxal; drug delivery

HIDROLISIS ENZIMATIK KITOSAN DENGAN KOMBINASI ENZIM ENDO-GLUCANASE DAN CELLOBIOHYDROLASE Nur Rokhati; Bambang Pramudono; Titik Istirokhatun; Mohammad Sulchan; Dyah Ayu Kresnianingrum; Luthfi Kurnia Dewi
Reaktor Volume 15 No.4 Oktober 2015
Publisher : Dept. of Chemical Engineering, Diponegoro University

Abstract CHITOSAN ENZYMATIC HYDROLYSIS USING A COMBINATION OF ENDO-GLUCANASE AND CELLOBIOHYDROLASE. Chitosan is very promising in various fields including medicine, pharmacology, and the food industry. However, the application of this polysaccharide is limited by its high molecular weight resulting in its low solubility in aqueous media. In this respect, the chitosan with shorter chain length, display a reduced viscosity and are soluble in aqueous media at pH values close to neutrality. The aim of this study is the hydrolysis of chitosan to obtain a low molecular weight chitosan using enzymes endo-glucanase and cellobiohydrolase. The hydrolysis of chitosan was carried out under a temperature of 40° C and pH 5. Chitosan degradation was monitored by the analysis of reducing sugars and viscosity, whereas the chemical characterization of chitosan is done by using test FTIR (infrared spectroscopy). The results showed that enzyme treatment resulted in a substantial loss in viscosity of the chitosan solution shows depolymerization. Depolymerization using endo-glucanase took place very quickly during the initial 15 minutes. The rate of viscosity decrease on chitosan degradation using cellobiohydrolase is lower than using endo-glucanase. When the reaction time was 4 h, the lowest viscosity is showed by cellobiohydrolase, and the highest solubility is showed by combination of endo-glucanase and cellobiohydrolase. Keywords: endo-glucanase; cellobiohydrolase; chitosan; hydrolysis Abstrak Kitosan dapat dimanfaatkan di berbagai bidang seperti kedokteran, farmasi dan industri makanan. Aplikasi kitosan sering dibatasi oleh berat molekul kitosan yang tinggi sehingga viskositasnya tinggi dan kelarutannya rendah. Kitosan dengan rantai polimer pendek, akan mempunyai viskositas rendah, dan mudah larut pada larutan/air dengan pH mendekati netral. Penelitian ini bertujuan untuk menghidrolisis kitosan secara enzimatis menggunakan enzim endo-glucanase dan cellobiohydrolase. Hidrolisis kitosan dilakukan pada suhu 40 °C dan pH 5. Degradasi kitosan dipantau melalui analisa gula reduksi dan viskositas, sedangkan karakterisasi kimia kitosan dilakukan dengan menggunakan uji FTIR (infra red spectroscopy). Hasil penelitian menunjukkan bahwa hidrolisis enzimatis kitosan dapat menyebabkan terjadinya penurunan berat molekul yang ditandai dengan adanya penurunan viscositas larutan kitosan. Pada 15 menit awal hidrolisis terjadi penurunan viskositas yang sangat besar. Laju penurunan viskositas enzim cellobiohydrolase lebih rendah dibanding dengan enzime endo-glucanase. Setelah waktu reaksi 4 jam, viskositas terendah diperoleh pada enzime cellobiohydrolase, sedangkan kelarutan tertinggi diperoleh pada kombinasi enzime endo-glucanase dan cellobiohydrolase. Kata kunci: endo-glucanase; cellobiohydrolase; kitosan; hidrolisis

Membrane Technology Application for Fractionation Process to Obtain High Quality Glucosamine Nur Rokhati; Titik Istirokhatun; Nur ‘Aini Hamada; Dwi Titik Apriyanti
Reaktor Volume 20 No.2 June 2020
Publisher : Dept. of Chemical Engineering, Diponegoro University

Glucosamine, monosaccharide from chitosan obtained from the chitin deacetylation process, has been used widely in various fields such as nutrition, pharmacy, and cosmetics. Glucosamine can be obtained from the hydrolysis of chitosan. Enzymatic hydrolysis provides the advantage of mild reaction conditions, environmentally friendly, and high yield. But until now, the separation of glucosamine from the chitosan hydrolysis fraction has been an obstacle. Ultrafiltration membranes offer an efficient filtration process because they do not require additional chemicals. The performance of ultrafiltration membranes was analyzed from the fractionation process of chitosan hydrolysis. The PES membranes in 10, 25, and 50 kDa were used to filter hydrolyzed Low Molecular Weight Chitosan (LMWC) in varied concentrations. The experiment was carried out in crossflow membrane module for flat sheet at room temperature in 1 bar. The permeate flux during filtration decreased rapidly at the initial and gradually over time because of fouling and concentration polarization. The more concentrated hydrolyzed LMWC solution resulted higher percentage of rejection up to almost 20% at the same membrane MWCO while higher MWCO resulted lower rejection percentage for the same hydrolyzed LMWC concentration. The FTIR spectrum of the used membranes of all types had absorption bands of glucosamine which proved that the fractionation process occurred. The time retention in HPLC chromatograms of glucosamine produced were similar with standard glucosamine. Thus, ultrafiltration could be applied for hydrolyzed LMWC fractionation process.Keywords: fractionation; glucosamine; LMWC; MWCO; ultrafiltration

PEMBUATAN RESIN PHENOL FORMALDEHID TERHADAP APLIKASINYA SEBAGAI VERNIS Nur Rokhati; Aji Prasetyaningrum
Reaktor Volume 12, Nomor 1, Juni 2008
Publisher : Dept. of Chemical Engineering, Diponegoro University

Phenol formaldehid termasuk kelompok resin sintetis yang dihasilkan dari reaksi polimerisasi antara phenol dengan formaldehid. Ada dua jenis resin phenol formaldehid yaitu : novolak yang bersifat termoplast dan resol yang bersifat termoset. Phenol formaldehid dapat diaplikasikan sebagai vernis karena dapat membentuk lapisan film yang kering.Penelitian dilakukan dengan mereaksikan phenol dan formaldehid dengan pH dan perbandingan mol bervariasi. Jenis novolak dibuat pada suasana asam dengan penambahan HCl, suhu 900C, dan waktu reaksi 5 jam, sedangkan jenis resol dibuat pada suasana basa dengan penambahan NaOH, suhu 800C dan waktu reaksi 3 jam. Hasil resin phenol formaldehid diaplikasikan sebagai vernis pada kayu jati. Hasil penelitian menunjukkan bahwa dengan bertambahnya pH dan perbandingan reaktan, waktu kering semakin lama. Kondisi optimum jenis novolak diperoleh pada pH 2,5 dan perbandingan reaktan 1 : 0,8, sedangkan untuk jenis resol dicapai pada pH 10 dan perbandingan mol reaktan 1 : 2. Aplikasi jenis novolak sebagai vernis kayu menghasilkan warna yang lebih cerah (tingkat gloss tinggi) dibanding dengan jenis resol

PENGARUH DERAJAT DEASETILASI KHITOSAN DARI KULIT UDANG TERHADAP APLIKASINYA SEBAGAI PENGAWET MAKANAN Nur Rokhati
Reaktor Volume 10, Nomor 2, Desember 2006
Publisher : Dept. of Chemical Engineering, Diponegoro University

Industri pengolahan udang banyak menimbulkan hasil samping berupa limbah kulit udang yang belum dimanfaatkan secara optimal, yaitu hanya dijadikan tepung dan campuran makanan ternak. Hal itu kurang memiliki nilai ekonomis dibandingkan dengan mengolahnya menjadi khitin dan khitosan. Khitosan banyak digunakan di berbagai industri. Salah satu penerapan khitosan yang penting dan dibutuhkan dewasa ini adalah sebagai pengawet bahan makanan pengganti formalin. Kualitas khitosan sering dinyatakan dengan besarnya nilai derajad deasetilasi. Penelitian ini bertujuan untuk menentukan kondisi operasi optimum proses deasetilasi khitin serta mempelajari pengaruh derajat deasetilasi terhadap khitosan sebagai bahan pengawet makanan. Proses deproteinisasi dengan larutan NaOH (3.5 % w/v) selama 2 jam pada suhu 65 oC dan proses demineralisasi dalam larutan HCl (1N) selama 30 menit pada suhu kamar. Proses deasetilasi dilakukan dengan memanaskan khitin dengan larutan NaOH (20%, 30%, 40%, 50%, 60%, 70%, 80% w/v) pada suhu (50 oC, 60 oC, 70 oC, 80 oC, 90 oC, 100 oC, 110 oC) selama (1, 2, 3, 4, 5, 6, 7 jam). Parameter respon adalah derajat deasetilasi khitosan. Produk khitosan diaplikasikan untuk pengawet tahu dan analisa mikroba dilakukan dengan menggunakan metode TPC untuk mengetahui pengaruh derajat deasetilasi terhadap kemampuannya mengawetkan makanan. Hasil penelitian menunjukkan bahwa kondisi optimum proses deasetilasi khitin menjadi khitosan adalah pada konsentrasi NaOH 50% dan suhu 100oC selama 1 jam yang memberikan derajat deasetilasi sebesar 71,2%.. Total bakteri pada perendaman tahu selama 3 hari dalam larutan asam asetat ditambah chitosan 6,8.104, dalam larutan asam asetat saja 9,9. 105, dan dalam blangko 8,6. 107, sehingga bisa disimpulkan bahwa khitosan dapat menghambat pertumbuhan bakteri. Namun meningkatnya derajad deasetilasi tidak begitu berpengaruh terhadap penurunan jumlah bakteri.

KARAKTERISASI FILM KOMPOSIT ALGINAT DAN KITOSAN Nur Rokhati; Bambang Pramudono; Nyoman Widiasa; Heru Susanto
Reaktor Volume 14, Nomor 2, Oktober 2012
Publisher : Dept. of Chemical Engineering, Diponegoro University

CHARACTERIZATION OF ALGINATE AND CHITOSAN COMPOSITE FILM. Due to the specific characteristics of (thin) films, the use of polymer films in various aplications has singnificantly increased. Alginate and chitosan are natural polymers, which have potential as a raw material for the manufacture of composite films. This paper presents the preparation and characterization of alginate, chitosan and chitosan-alginate composite films. The film characterization included permeability test, degree of swelling, mechanical property, morphology (by SEM), and surface chemistry (by FTIR). The results showed that alginate films have a higher permeability and degree of swelling (DS) than chitosan films. Both permeability and DS decreased with increasing concentration for both alginate and chitosan films. DS experiments showed that the films have the highest DS in water followed by ethanol 95% and ethanol >99.9%, respectively. The mechanical strength of chitosan films was larger than alginate films. Alginate-chitosan composite films prepared by layer by layer method showed better characteristics than the composite films prepared by blending of alginate and chitosan solutions. Meningkatnya aplikasi film polimer di berbagai industri tidak terlepas dari keunggulan yang dimiliki. Alginat dan kitosan merupakan polimer alam yang mempunyai potensi sebagai bahan dasar pembuatan film komposit. Pada penelitian ini dilakukan pembuatan dan karakterisasi film komposit berbasis alginat dan kitosan. Karakterisasi film yang dilakukan meliputi uji: permeabilitas, derajat swelling, mekanik, morfologi (dengan SEM), dan struktur kimia permukaan (dengan FTIR). Hasil penelitian menunjukkan bahwa film alginat mempunyai nilai permeabilitas maupun derajat swelling yang lebih tinggi dibanding dengan film kitosan. Baik pada kitosan maupun alginat memberikan fenomena bahwa semakin besar konsentrasi larutan maka semakin kecil nilai permeabilitas maupun derajat swelling, dengan derajat swelling terhadap air adalah yang paling besar kemudian diikuti oleh ethanol teknis (± 95%) dan yang terkecil adalah ethanol PA (> 99,9%). Kekuatan mekanik film kitosan lebih besar dibanding dengan film alginat. Film komposit alginat-kitosan yang dibuat dengan metode layer by layer memberikan karakteristik yang lebih baik dibanding dengan film komposit yang dibuat dengan pencampuran larutan alginat dan larutan kitosan.

Influence of Microwave Irradiation on Extraction of Chitosan from Shrimp Shell Waste Dwi Titik Apriyanti; Heru Susanto; Nur Rokhati
Reaktor Volume 18 No. 1 March 2018
Publisher : Dept. of Chemical Engineering, Diponegoro University

Chitosan is natural polysaccharides which is nontoxic, biodegradable, and biocompatible and have many advantages in various kinds of fields including health, food, agriculture, and industry. Chitosan usually take long time to extract by conventional method for deacetylation process of chitin. Raw material for chitosan can be found in shrimp shell waste. Chitosan manufactures usually need high temperatures and chemicals in large quantities and it takes much time and consumes a lot of energy where will give bad effect to the environment. Recently microwave irradiation as nonconventional energy sources is widely used in chemical reactions. To reduce the impact of environmental pollution due to excessive use of chemical treatment, the objective of this work is processing chitosan under microwave irradiation. Expected production of chitosan with the same mass requires fewer chemicals than conventional heating. In particular, the study will examine the effect of making the chitosan and adding chemicals, reaction time and operating temperature and degree of deacetylation in chitosan with conventional heating methods that the results will be compared using a microwave. In this research will be developed to the design and fabrication of prototype scale extractor for manufacturing chitosan from shrimp shell waste after optimum results obtained from the research laboratory scale. From the research we can conclude that microwave will speed up reaction time. FTIR also showed functional group of chitosan formed from microwave irradiation have same results. Keywords: chitosan, shrimp shells, microwave

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