STUDI ISOLASI DAN ESTERIFIKASI PATCHOULI ALKOHOL DARI MINYAK NILAM

Ika Yuliawati, Dr. Chairil Anwar

2014 | Tesis | S2 Ilmu Kimia

Telah dilakukan isolasi dan esterifikasi patchouli alkohol (PA) dari minyak nilam. Patchouli alkohol merupakan komponen utama dalam minyak nilam. Penelitian diawali dengan memisahkan minyak nilam menjadi 3 fraksi menggunakan distilasi fraksinasi pengurangan tekanan. Patchouli alkohol dikristalisasi dari fraksi III (mengandung patchouli alkohol sebesar 78,91%) dengan penambahan bibit kristal. Fraksi III (108-116 oC) didinginkan -22 oC selama 12 hari. Kristal patchouli alkohol ditentukan titik lelehnya dan dikarakterisasi 1H-NMR. Patchouli asetat disintesis dari reaksi esterifikasi patchouli alkohol, asam asetat glasial dan katalis H2SO4 pekat pada suhu 50-52 oC selama 3 jam dan sonikasi variasi waktu reaksi 1, 2 dan 3 jam. Kristal patchouli alkohol yang dihasilkan sebesar 55,88% dengan kemurniannya € 99%. Titik leleh kristal 52,10-55.70 oC. Data spektra 1H-NMR patchouli alkohol hasil isolasi adalah  1,94-1,77 (3H, m), 1,70-1,66 (1H, m), 1,48-1,20 (7H, m), 1,15 (1H, s, OH), 1,04 (6H, d, J 5,15 Hz), 0,81 (1H, s, CH3- tersier), 0,76 (3H, d, J 7,17 Hz, CH3-sekunder). Patchouli asetat dari reaksi esterifikasi patchouli alkohol pada suhu 50-52 oC selama 3 jam sebesar 53,58% dan sonikasi variasi waktu 1, 2 dan 3 jam secara berurutan sebesar 17,92; 3,71 dan 3,25%. Kata kunci : Isolasi, kristalisasi, patchouli alkohol, patchouli asetat, sonikasi

Isolation and esterification of patchouli alcohol (PA) from patchouli oil has been conducted. Patchouli alcohol is the major constituent of patchouli oil. The first step of research, patchouli oil was separated into three fractions using fractional distillation under reduced pressure. Patchouli alcohol was crystallized from fraction III (containing 78.91% PA) using seeding method. Fraction III (108-116 oC) was cooled at -22 oC for 12 days. Crystal patchouli alcohol was determined its melting point (MP) and was characterized 1H-NMR. Patchouli acetate was synthesized by esterification of patchouli alcohol, acetic acid and H2SO4 catalyst at 50-52 oC for 3 h and sonication for 1, 2 and 3 h. Patchouli alcohol crystal obtained was 55.88% with >99% purity. The melting point of crystal was 52.10-55.70 oC. The 1H-NMR spectra data were  1.94-1.77 (3H, m), 1.70-1.66 (1H, m), 1.48-1.20 (7H, m), 1.15 (1H, s, OH), 1.04 (6H, d, J 5.15 Hz), 0.81 (1H, s, tert-CH3), 0.76 (3H, d, J 7.17 Hz, sec-CH3). Patchouli acetate by esterification patchouli alcohol at 50-52 oC for 3 h is 53.58% and sonication for 1, 2 and 3 h is 17.92; 3.17 and 3.25%. Keywords : Isolation, crystallization, patchouli alcohol, patchouli acetate, sonication

Kata Kunci : Isolasi, kristalisasi, patchouli alkohol, patchouli asetat, sonikasi