Mustafiah, Mustafiah (2026) Ekstraksi Minyak Atsiri Dari Pala (Myristica Fragrans Houtt.) Dengan Metode Microwave Air-Hydrodistillation Dan Enkapsulasi. Doctoral thesis, Institut Teknologi Sepuluh Nopember.
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Abstract
Minyak atsiri pala (Myristica fragrans Houtt.) memiliki potensi luas sebagai bahan baku bernilai tambah dalam industri pangan, farmasi, kosmetik, dan kesehatan. Namun, proses ekstraksi menggunakan metode konvensional umumnya masih menghadapi beberapa keterbatasan, antara lain waktu ekstraksi yang relatif lama, kebutuhan energi yang tinggi, serta efisiensi perolehan minyak atsiri yang belum optimal. Penelitian ini bertujuan untuk mengembangkan proses ekstraksi minyak atsiri dari fuli dan biji pala menggunakan metode Microwave Air-Hydrodistillation (MAHD), mengkaji karakteristik fisikokimia dan aktivitas biologis minyak yang dihasilkan, mengoptimasi kondisi operasi ekstraksi, mengembangkan model kinetika ekstraksi, serta meningkatkan stabilitas minyak atsiri melalui proses mikroenkapsulasi. Ekstraksi dilakukan pada variasi daya microwave 300, 450, dan 600 W, rasio bahan terhadap pelarut 0,20; 0,25; dan 0,30 g/mL, ukuran partikel 20, 60, dan 1000 mesh, serta waktu ekstraksi mulai 20 hingga 180 menit. Optimasi proses dilakukan menggunakan Response Surface Methodology (RSM) dengan desain Box-Behnken (BBD). Karakterisasi minyak atsiri meliputi warna, aroma, bobot jenis, kelarutan dalam alkohol 90%, komposisi kimia menggunakan GC-MS, aktivitas antioksidan, dan aktivitas antibakteri. Minyak atsiri yang diperoleh selanjutnya dienkapsulasi menggunakan matriks kitosan–maltodekstrin melalui proses emulsifikasi, crosslinking dengan sodium tripolyphosphate (STPP), dan freeze drying. Mikrokapsul yang dihasilkan dievaluasi berdasarkan yield, ukuran partikel, profil pelepasan (release) dan kinetika pelepasan terkontrol (controlled release). Hasil penelitian menunjukkan bahwa kondisi optimum ekstraksi minyak atsiri fuli pala diperoleh pada daya microwave 450–600 W, rasio bahan terhadap pelarut 0,30 g/mL, dan ukuran partikel 60 mesh dengan yield sebesar 10,71%. Sementara itu, kondisi optimum ekstraksi minyak atsiri biji pala diperoleh pada daya microwave 600 W, rasio bahan terhadap pelarut 0,30 g/mL, dan ukuran partikel 100 mesh dengan yield sebesar 6,36%. Komponen utama minyak atsiri fuli pala terdiri atas methyl eugenol (16,89%), terpinen-4-ol (10,13%), myristicin (9,32%), eugenol (8,63%), dan safrole (8,13%), sedangkan minyak atsiri biji pala didominasi oleh 4-terpineol (29,45%), myristicin (15,64%), eugenol (7,76%), dan estragole (5,89%). Aktivitas antioksidan minyak atsiri fuli pala menunjukkan nilai IC50 sebesar 1,14 mg/mL. Uji antibakteri menunjukkan bahwa minyak atsiri fuli dan biji pala mampu menghambat pertumbuhan Escherichia coli (Gram-negatif) dengan daya hambat kuat hingga 168 jam dan Staphylococcus aureus (Gram-positif) dengan daya hambat kuat hingga 192 jam. Analisis kinetika menunjukkan bahwa secara umum model Weibull menunjukkan performa paling konsisten di semua daya microwave dengan R² 0.9955 dan RMSE terendah 0.0303 untuk biji pala. Pada minyak atsiri fuli pala, Weibull unggul pada daya 300–450 W (R² 0.9964; RMSE 0.0104), tetapi pada kondisi tertentu pada daya 600 W, Power Law paling akurat (R² 0.9989; RMSE 0.0087) menggambarkan ekstraksi cepat dan intensif. Pada tahap mikroenkapsulasi, kondisi optimum diperoleh pada rasio bahan penyalut kitosan:maltodekstrin 0,01:1. Pada kondisi tersebut, yield mikrokapsul tertinggi dicapai sebesar 67,97% untuk minyak atsiri fuli pala dan 65,82% untuk minyak atsiri biji pala. Mikrokapsul fuli pala memiliki ukuran partikel rata-rata 919,3 nm dengan distribusi yang lebih homogen (RSD 13,36%), sedangkan mikrokapsul biji pala memiliki ukuran partikel rata-rata 632,3 nm dengan distribusi yang lebih heterogen (RSD 40,68%). Sistem mikroenkapsulasi mampu menurunkan laju pelepasan minyak atsiri secara signifikan, dengan nilai release maksimum hanya sekitar 7–8% selama 182 jam, sedangkan pada minyak atsiri yang tidak terenkapsulasi sekitar 25,89–53,86%, sehingga menunjukkan kemampuan yang baik dalam meningkatkan stabilitas dan menghasilkan pelepasan terkendali (controlled release). Untuk kinetika pelepasan, model kinetika orde satu paling sesuai untuk menggambarkan profil pelepasan minyak atsiri fuli pala dan biji pala, baik dalam bentuk bebas maupun terenkapsulasi. Secara keseluruhan, metode MAHD terbukti efektif untuk menghasilkan minyak atsiri pala dengan kualitas yang memenuhi standar dan waktu proses yang lebih efisien dibandingkan dengan metode konvensional. Kombinasi optimasi proses, pemodelan kinetika, dan mikroenkapsulasi berbasis kitosan–maltodekstrin memberikan pendekatan yang menjanjikan untuk meningkatkan nilai tambah dan stabilitas minyak atsiri pala pada berbagai aplikasi industri.
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Nutmeg (Myristica fragrans Houtt.) essential oil has broad potential as a value-added raw material for the food, pharmaceutical, cosmetic, and health-related industries. However, conventional extraction methods commonly face several limitations, including relatively long extraction times, high energy demand, and suboptimal essential oil recovery. This study aimed to develop an extraction process for essential oils from nutmeg mace and seeds using Microwave Air-Hydrodistillation (MAHD), evaluate the physicochemical characteristics and biological activities of the extracted oils, optimize the extraction operating conditions, develop extraction kinetic models, and improve essential oil stability through microencapsulation. Extraction was carried out at microwave powers of 300, 450, and 600 W; feed-to-solvent ratios of 0.20, 0.25, and 0.30 g/mL; particle sizes of 20, 60, and 100 mesh; and extraction times ranging from 20 to 180 min. Process optimization was performed using Response Surface Methodology (RSM) with a Box–Behnken Design (BBD). Essential oil characterization included color, aroma, specific gravity, solubility in 90% alcohol, chemical composition using GC–MS, antioxidant activity, and antibacterial activity. The obtained essential oils were subsequently encapsulated using a chitosan–maltodextrin matrix through emulsification, crosslinking with sodium tripolyphosphate (STPP), and freeze drying. The resulting microcapsules were evaluated based on yield, particle size, release profile, and controlled-release kinetics. The results showed that the optimum extraction condition for nutmeg mace essential oil was obtained at a microwave power of 450–600 W, a feed-to-solvent ratio of 0.30 g/mL, and a particle size of 60 mesh, resulting in a yield of 10.71%. Meanwhile, the optimum extraction condition for nutmeg seed essential oil was achieved at a microwave power of 600 W, a feed-to-solvent ratio of 0.30 g/mL, and a particle size of 100 mesh, resulting in a yield of 6.36%. The major components of nutmeg mace essential oil were methyl eugenol (16.89%), terpinen-4-ol (10.13%), myristicin (9.32%), eugenol (8.63%), and safrole (8.13%), whereas nutmeg seed essential oil was dominated by 4-terpineol (29.45%), myristicin (15.64%), eugenol (7.76%), and estragole (5.89%). The antioxidant activity of nutmeg mace essential oil showed an IC50 value of 1.14 mg/mL. Antibacterial testing demonstrated that both nutmeg mace and seed essential oils were able to inhibit the growth of Escherichia coli (Gram-negative) with strong inhibition for up to 168 h and Staphylococcus aureus (Gram-positive) with strong inhibition for up to 192 h. Kinetic analysis showed that, in general, the Weibull model provided the most consistent performance across all microwave powers, with R² ≥ 0.9955 and the lowest RMSE of 0.0303 for nutmeg seed. For nutmeg mace essential oil, the Weibull model was superior at 300–450 W (R² ≥ 0.9964; RMSE 0.0104); however, under certain conditions at 600 W, the Power Law model was the most accurate (R² = 0.9989; RMSE = 0.0087) in describing rapid and intensive extraction. In the microencapsulation stage, the optimum condition was obtained at a chitosan-to-maltodextrin wall material ratio of 0.01:1. Under this condition, the highest microcapsule yields were 67.97% for nutmeg mace essential oil and 65.82% for nutmeg seed essential oil. Nutmeg mace microcapsules had an average particle size of 919.3 nm with a more homogeneous distribution (RSD 13.36%), whereas nutmeg seed microcapsules had an average particle size of 632.3 nm with a more heterogeneous distribution (RSD 40.68%). The microencapsulation system significantly reduced the release rate of the essential oils, with a maximum release of only approximately 7–8% over 182 h, compared with approximately 25.89–53.86% for the non-encapsulated essential oils. This indicates the ability of the system to improve stability and provide controlled release. In terms of release kinetics, the first-order kinetic model was the most suitable for describing the release profiles of both nutmeg mace and seed essential oils, either in free or encapsulated form. Overall, the MAHD method proved effective in producing nutmeg essential oil with quality that met the required standards and with a more efficient processing time compared with conventional methods. The combination of process optimization, kinetic modeling, and chitosan–maltodextrin-based microencapsulation provides a promising approach to enhancing the added value and stability of nutmeg essential oil for various industrial applications.
| Item Type: | Thesis (Doctoral) |
|---|---|
| Uncontrolled Keywords: | Myristica fragrans Houtt., Microwave Air-Hydrodistillation, minyak atsiri, optimasi, kinetika ekstraksi, mikroenkapsulasi, freeze drying. Controlled release.; Myristica fragrans Houtt.; Microwave Air-Hydrodistillation; essential oil; optimization; extraction kinetics; microencapsulation; freeze drying; controlled release. |
| Subjects: | H Social Sciences > HD Industries. Land use. Labor > HD9490.A2 Essences and essential oils industry. T Technology > TP Chemical technology > TP156 Crystallization. Extraction (Chemistry). Fermentation. Distillation. Emulsions. T Technology > TP Chemical technology > TP248.25.N35 Microencapsulation. |
| Divisions: | Faculty of Industrial Technology and Systems Engineering (INDSYS) > Chemical Engineering > 24001-(S3) PhD Thesis |
| Depositing User: | Mustafiah Mustafiah |
| Date Deposited: | 29 Jul 2026 01:26 |
| Last Modified: | 29 Jul 2026 01:26 |
| URI: | http://repository.its.ac.id/id/eprint/139147 |
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