Danissa, Hanum Ardhyni (2021) Isolasi dan Pemurnian SenyawaSqualene pada Daun Nyamplung(Calophyllum inophyllum). Masters thesis, Institut Teknologi Sepuluh Nopember.
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Abstract
Squalene merupakan senyawa bioaktif yang terdapat pada daun nyamplung. Studi melaporkan bahwa mengkonsumsi minyak sehat yang mengandung squalene lebih banyak mampu mengurangi penyakit kardiovaskular dan kanker. Penelitihan ini bertujuan untuk mengisolasi dan memurnikan senyawa squalene pada daun nyamplung. Pertama, daun nyamplung dihaluskan dan diekstraksi menggunakan metode Solid-Liquid Extraction (SLE) dengan heksana atau metanol kemudian masing-masing hasil ekstraksi dianalisa Gas Chromatography (GC) untuk menentukan kandungan squalene. Setelah diketahui crude heksana memiliki kandungan squalene yang tinggi dilakukan proses pemisahan dengan beberapa metode yaitu batchwise solvent extraction (BSE) dengan pengulangan metanol, metode batchwise solvent extraction (BSE) dengan pengulangan heksana, dan metode multistage adsorption-desorption (MAD). Pada metode BSE dengan pengulangan metanol, 1 gram crude heksana dilarutkan dengan 200mL heksana lalu ditambahkan 50mL metanol. Setelah 1 jam, fraksi methanol (PF) dipisahkan dari fraksi heksana (NPF) kemudian untuk NPF ditambahkan dengan metanol baru 50mL hingga stage ke 5. Sedangkan untuk metode BSE dengan pengulangan heksana sama dengan sebelumnya tetapi 1 gram crude heksana dilarutkan ke dalam 50mL metanol. Kemudian ditambahkan dengan heksana 50mL. Setelah 1jam, fraksi heksana (NPF) dipisahkan dari fraksi metanol (PF) kemudian fraksi metanol ditambahkan dengan heksana 50mL hingga stage ke 10. Hasil dari fraksi heksana diuapkan dan dikumpulkan dari pelarutnya menjadi fraksi non-polar (NPF mix). Untuk metode MAD dilakukan dengan 2 suhu yang berbeda yaitu 3 dan 30°C. Perbandingan massa silika gel terhadap crude heksana adalah 1:1; 2:1; dan 4:1 (m/m). Selanjutnya, fraksi n-heksana dipisahkan dari silika gel dengan penyaringan. Fraksi N-heksana ditetapkan sebagai fraksi non-polar (NPF), sedangkan fraksi silika gel ditetapkan sebagai fraksi polar (PF). PF berwarna gelap digunakan untuk proses desorpsi menggunakan metanol sampai warnanya menjadi tidak berwarna. Sedangkan NPF diekstraksi dengan silika gel baru hingga mencapai stage 10. NPF dan PF masing-masing metode dianalisis secara kuantitatif dan kualitatif masing-masing menggunakan Thin Layer Chromatography (TLC) dan GC. Didapatkan kondisi terbaik pada metode MAD suhu 30°C, variabel 1:1 (m/m), pada stage ke 9 dengan kemurnian awal squalene 11,03% menjadi 67,42%. dan recovery 40,01%.
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Squalene is a bioactive compound found in nyamplung leaves. Studies report that consuming healthy oils that contain more squalene can reduce cardiovascular disease and cancer. This study aims to isolate and purify squalene compounds in nyamplung leaves. First, nyamplung leaves were ground and extracted using the Solid-Liquid Extraction (SLE) method with hexane or methanol, and then each extraction result was analyzed by Gas Chromatography (GC) to determine the squalene content. After knowing that crude hexane has a high squalene content, the separation process is carried out using several methods, namely batchwise solvent extraction (BSE) with methanol repetition, batchwise solvent extraction (BSE) method with hexane repetition, and multistage adsorption-desorption (MAD) method. In the BSE method with repeated methanol, 1 gram of crude hexane is dissolved in 200mL of hexane and then 50mL of methanol is added. After 1 hour, the methanol fraction (PF) was separated from the hexane fraction (NPF) then NPF was added with 50mL of new methanol to stage 5. As for the BSE method with the same hexane repetition as before but 1 gram of crude hexane was dissolved in 50mL of methanol. Then added with 50 mL of hexane. After 1 hour, the hexane fraction (NPF) was separated from the methanol fraction (PF) then the methanol fraction was added with 50 mL hexane to stage 10. The results from the hexane fraction were evaporated and collected from the solvent into a non-polar fraction (NPF mix). The MAD method is carried out at 2 different temperatures, namely 3 and 30°C. The mass ratio of silica gel to crude hexane is 1:1; 2:1; and 4:1 (m/m). Next, the n-hexane fraction was separated from the silica gel by filtration. The N-hexane fraction was designated as the non-polar fraction (NPF), while the silica gel fraction was designated as the polar fraction (PF). Dark-colored PF was used for the desorption process using methanol until the color became colorless. Meanwhile, NPF was extracted with new silica gel until it reached stage 10. NPF and PF were analyzed quantitatively and qualitatively using Thin Layer Chromatography (TLC) and GC, respectively. The best conditions were obtained in the MAD method at 30°C, variable 1:1 (m/m), at stage 9 with an initial purity of 11.03% to 67.42%. and 40.01% recovery.
Item Type: | Thesis (Masters) |
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Uncontrolled Keywords: | adsorpsi, batchwise solvent extraction, desoprpsi, nyamplung, senyawa bioaktif, silika gel, squalene,adsorption, silica gel, desorption |
Subjects: | Q Science > QD Chemistry > QD471 Chemical compounds - Structure and formulas Q Science > QD Chemistry > QD63 Extraction |
Divisions: | Faculty of Industrial Technology > Chemical Engineering > 24101-(S2) Master Thesis |
Depositing User: | Danissa Hanum Ardhyni |
Date Deposited: | 20 Aug 2021 05:51 |
Last Modified: | 20 Aug 2021 05:51 |
URI: | http://repository.its.ac.id/id/eprint/87997 |
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