Muhammad Usman, Sihab and Dr. Dodyk Pranowo,, STP, M.Si. and Prof. Dr. Ir. Imam Santoso,, MP. (2023) Optimasi Ekstraksi Nanokalsium dengan Ultrasonik dari Tulang Ikan Tenggiri (Scomberomorus sp.) dan Karakterisasi Hidroksiapatit dengan Sintesis Sol-Gel. Sarjana thesis, Universitas Brawijaya.
Abstract
Kalsium merupakan mineral esensial yang memiliki peranan penting di dalam tubuh untuk pembentukan tulang. Kalsium umum dikonsumsi terdapat dalam bentuk mikro kalsium. Ukuran tersebut terkait dengan besarnya penyerapan kalsium oleh tubuh, biasanya hanya 50% sehingga sering menyebabkan defisiensi. Sumber kalsium yang aman digunakan umumnya dari tulang ikan, yang merupakan limbah tidak termanfaatkan. Salah satu tulang ikan yang dapat dimanfaatkan sebagai sumber kalsium yaitu dari tulang ikan tenggiri. Kalsium berukuran nano lebih mudah diserap oleh tubuh dan dapat terapsorbsi secara cepat dan sempurna. Ultrasound-Assisted Extraction (UAE) merupakan salah satu novel technology yang dapat digunakan untuk mengekstrak nanokalsium. Penelitian terdiri dari dua tahapan, tahap pertama adalah optimasi ekstraksi nanokalsium dari tulang ikan tenggiri dengan UAE dan tahap kedua adalah sintesis hidroksiapatit (HAp) dengan metode sol-gel. Tujuan penelitian ini adalah untuk menganalisis interaksi waktu eksitasi dan amplitudo terhadap respon (rendemen, derajat putih, kadar kalsium dan kadar fosfor) serta menganalisis karakteristik HAp yang dihasilkan dari sintesis sol-gel. Kualitas ekstrak nanokalsium dioptimasi dengan metode Response Surface Methodology (RSM). Verifikasi respon optimal dilakukan dengan 3 kali pengulangan dan dilakukan uji proksimat, XRD, FTIR, dan SEM-EDX. HAp yang dihasilkan dari sintesis sol-gel dikarakterisasi dengan uji XRD, FTIR, dan SEM-EDX. Hasil penelitian diketahui bahwa kondisi optimal untuk ekstraksi nanokalsium menggunakan waktu eksitasi 111,149 menit dan amplitudo 75% menghasilkan respon rendemen 48,129%, derajat putih 82,940%, kadar kalsium 48,844% dan kadar fosfor 8,882%. Karakterisasi nanokalsium dengan pengujian ukuran partikel dihasilkan ukuran rata-rata 142,3 nm. Hasil analisa XRD menunjukkan puncak utama muncul pada sudut 2θ = 31,73° dengan intensitas 223,11, ukuran rata-rata kristal 26,16 nm dan derajat kristalinitas sebesar 83,35%. Morfologi permukaan sampel nanokalsium berbentuk bongkahan yang menunjukkan karakter poliskistalin dari nanopartikel CaO. Analisis EDS menunjukkan unsur Ca dan O yang dominan dengan masing-masing 31,60% dan 34,17%. Analisis gugus fungsi yang terindikasi pada nanokalsium diantaranya adalah gugus fosfat (PO 4 3- ), karbonat (CO 3 2- ), dan hidroksil (OH). Hasil karakterisasi XRD sintesis hidroksiapatit dengan prekursor nanokalsium menunjukkan puncak utama pada sudut 2θ = 42,67° dengan intensitas 624,32. Peak dengan intensitas tersebut disesuaikan database Match®! dan didapat senyawa hidroksiapatit-dental. Berdasarkan persamaan scherrer diperoleh ukuran rata-rata kristal 44,73 nm dengan derajat kristalinitas 92,96%. Analisis EDS menunjukkan komposisi unsur hidroksiapatit hasil sintesis didominasi oleh unsur Ca, P, O, dan C. Berdasarkan data analisis EDS, didapatkan rasio Ca/P hidroksiapatit hasil sintesis sebesar 2,03 yang termasuk dalam carbonated-HAp dengan rasio Ca/P 1,86-2,08.
English Abstract
Calcium is an essential mineral that has an important role in the body for bone formation. Calcium is commonly consumed in the form of micro calcium. This size is related to the amount of calcium absorption by the body, usually only 50%, so it often causes deficiency. A safe source of calcium is generally from fish bones, which are unutilized waste. One of the fish bones that can be used as a source of calcium is from mackerel fish bones. Nano-sized calcium is more easily absorbed by the body and can be absorbed quickly and completely. Ultrasound-Assisted Extraction (UAE) is a novel technology that can be used to extract nanocalcium. The research consisted of two stages, the first stage was optimization of nanocalcium extraction from mackerel bones with UAE and the second stage was the synthesis of hydroxyapatite (HAp) using the sol-gel method. The aims of this study were to analyze the interaction between excitation time and amplitude on response (yield, whiteness, calcium and phosphorus levels) and to analyze the characteristics of the HAp produced from sol-gel synthesis. The quality of the nanocalcium extract was optimized using the Response Surface Methodology (RSM) method. Optimal response verification was carried out with 3 repetitions and proximate tests, XRD, FTIR, and SEM-EDX were performed. HAp produced from sol-gel synthesis was characterized by XRD, FTIR, and SEM-EDX tests. The results showed that the optimal conditions for nanocalcium extraction using an excitation time of 111.149 minutes and an amplitude of 75% resulted in a yield response of 48.129%, degree of whiteness of 82.940%, calcium content of 48.844% and phosphorus content of 8.882%. Characterization of nanocalcium by testing the particle size resulted in an average size of 142.3 nm. The results of the XRD analysis showed that the main peak appeared at an angle of 2θ = 31.73° with an intensity of 223.11, an average crystal size of 26.16 nm and a degree of crystallinity of 83.35%. The surface morphology of the nanocalcium sample is in the form of chunks which shows the polycystalline character of the CaO nanoparticles. EDS analysis showed that Ca and O were dominant with 31.60% and 34.17% respectively. Analysis of the functional groups indicated in nanocalcium include phosphate (PO 4 3- ), carbonate (CO 3 2- ), and hydroxyl (OH) groups. The results of the XRD characterization of the synthesis of hydroxyapatite with nanocalcium precursors showed the main peak at an angle of 2θ = 42.67° with an intensity of 624.32. Peaks with these intensities are adjusted to the Match®! database. and hydroxyapatite-dental compound was obtained. Based on the Scherrer equation, an average crystal size of 44.73 nm is obtained with a crystallinity degree of 92.96%. EDS analysis showed that the elemental composition of the synthesized hydroxyapatite was dominated by Ca, P, O, and C. Based on the EDS analysis data, the Ca/P hydroxyapatite ratio synthesized was 2.03 which is included in carbonated-HAp with a Ca/P ratio of 1. 86-2.08.
| Item Type: | Thesis (Sarjana) |
|---|---|
| Identification Number: | 052310 |
| Uncontrolled Keywords: | Ultrasound-Assisted Extraction, Nanocalcium, Hydroxyapatite, SolGel Ultrasound-Assisted Extraction, Nanokalsium, Hidroksiapatit, Sol-Gel |
| Divisions: | Fakultas Teknologi Pertanian > Teknologi Industri Pertanian |
| Depositing User: | Unnamed user with username verry |
| Date Deposited: | 11 Jan 2024 07:41 |
| Last Modified: | 11 Jan 2024 07:41 |
| URI: | http://repository.ub.ac.id/id/eprint/208547 |
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