Syamsiyah, Siti (2025) Ekstraksi Minyak Atsiri Dari Daun Dan Biji Lada Putih (Piper nigrum L.) Menggunakan Metode Microwave Air Hydrodistillation. Masters thesis, Institut Teknologi Sepuluh Nopember.
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Abstract
Lada putih (Piper nigrum L.) merupakan rempah yang mengandung minyak atsiri, dengan rasa pedas dan aroma khas. Kalimantan Timur, dengan luas kebun 8.161 ha, menjadi salah satu sentra produksi lada putih. Ekstraksi minyak atsiri umumnya menggunakan distilasi konvensional yang memerlukan energi tinggi, pelarut organik, dan waktu lama. Untuk itu, digunakan metode microwave air hydrodistillation (MAHD) sebagai 'metode hijau' untuk mengekstraksi minyak atsiri dengan energi, pelarut, dan waktu yang minimum. Penelitian ini bertujuan mempelajari proses ekstraksi minyak atsiri dari daun dan biji lada putih, pengaruh ukuran bahan, daya microwave, dan waktu ekstraksi terhadap yield minyak atsiri, menentukan kondisi optimal mengunakan Response Surface Methodology (RSM) dengan model Box Bohnken Design (BBD), menentukan model kinetika ekstraksi dan mengatahui karakteristik minyak atsiri. Metode MAHD terdiri atas tiga komponen utama, yaitu microwave sebagai pemanas, kompresor untuk menginjeksikan udara ke dalam distiler, dan kondensor sebagai sistem pendingin. Pada penelitian ini, digunakan 50gram daun lada dengan variasi ukuran lebar daun (1 cm, 2 cm, dan 3 cm) yang ditambahkan 750 mL aquadest, serta 100gram biji lada putih dengan variasi ukuran partikel (lolos ayakan 60 mesh, 80 mesh, dan 100 mesh) yang ditambahkan 500 mL aquadest. Udara dari kompresor diinjeksikan ke dalam campuran bahan dan pelarut dengan laju alir 1 L/menit. Selanjutnya, campuran dipanaskan menggunakan microwave dengan variasi daya (300 W, 450 W, dan 600 W) hingga menghasilkan uap. Uap yang terbentuk kemudian dikondensasi menjadi distilat, yang terdiri atas dua fase minyak atsiri di bagian atas dan aquadest di bagian bawah. Distilat dikumpulkan setiap 20 menit selama proses ekstraksi berlangsung selama 180 menit. Hasil penelitian menunjukkan bahwa semakin kecil ukuran bahan dan semakin tinggi daya microwave meningkatkan yield minyak atsiri dengan durasi waktu ekstraksi 180 menit menggunakan metode MAHD. Yield tertinggi minyak atsiri daun lada sebesar 0,4288% (ukuran 1 cm, 600 W) dan biji lada putih sebesar 3,0018% (lolos 80 mesh, 600 W). Optimasi dengan metode RSM–BBD menghasilkan kondisi optimum ekstraksi minyak atsiri daun lada pada ukuran 1,021 cm, waktu 179,49 menit, dan daya 489,79 W (yield prediksi 0,410% dengan desirability 1). Untuk biji lada, optimum diperoleh pada ukuran 88,41 mesh, waktu 180 menit, dan daya 600 W (yield prediksi 2,967% dengan desirability 0,979). Model kinetika terbaik untuk daun lada mengikuti Power’s Law dengan R² = 0,9924–0,9965 dan RMSD = 0,0180–0,0281, sedangkan untuk biji lada mengikuti model Hyperbolic dengan R² > 0,999 dan RMSD = 0,0053–0,0076.
Hasil karakteristik minyak atsiri daun lada yaitu berwarna hijau, berat jenis 0,7999, indeks bias 1,4950, dan 1 mL minyak astiri larut dalam 10 mL etanol 95%, dengan senyawa utama β-Elemene (4,82%), (trans)-β-caryophyllene (2,25%), α-Humulene (2,00%), α-Selinene (6,13%), Germacrene-D (0,27%), isospathulenol (4,21%) dan neointermedeol (4,96%). Minyak atsiri biji lada berwarna hijau, berat jenis 0,8796, indeks bias 1,4845, dan 1 mL minyak atsiri larut dalam 4–5 mL etanol, dengan senyawa utama α-Pinene (3,65%), Δ-3-Carene (22,36%), D-Limonene (15,32%), β-Myrcene (2,54%), Bicyclo[3.1.1]heptane, 6,6-dimethyl-2-methylene-, (1S)- (8,20%), α-Humulene (2,23%), dan (trans)-β-Caryophyllene (18,05%). Anlisa Uji antibakteri terhadap Staphylococcus aureus menunjukkan zona hambat minyak daun sebesar 1,9005 mm (hari ke-1) dan 3,5160 mm (hari ke-5), sedangkan minyak biji menunjukkan 3,18791mm (hari ke-1) dan 3,7333 mm (hari ke-5).
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White pepper (Piper nigrum L.) is a spice that contains essential oil, characterized by its pungent taste and distinctive aroma. East Kalimantan, with a plantation area of 8,161 hectares, is one of the main production centers of white pepper. Essential oil extraction is generally carried out using conventional distillation, which requires high energy, organic solvents, and a long processing time. Therefore, the Microwave Air-Hydrodistillation (MAHD) method is used as a "green method" to extract essential oils with minimal energy, solvent, and time requirements. This study aimed to investigate the extraction process of essential oils from white pepper leaves and seeds, the effect of particle size, microwave power, and extraction time on oil yield, determine the optimal conditions using Response Surface Methodology (RSM) with Box-Behnken Design (BBD), model the extraction kinetics, and characterize the essential oils. The MAHD method consists of three main components: a microwave as the heating source, a compressor for injecting air into the distiller, and a condenser as the cooling system. In this study, 50 grams of white pepper leaves with varying leaf widths (1 cm, 2 cm, and 3 cm) were mixed with 750 mL of distilled water, while 100 grams of white pepper seeds with different particle sizes (passed through 60 mesh, 80 mesh, and 100 mesh sieves) were mixed with 500 mL of distilled water. Air was injected into the mixture of raw material and solvent at a flow rate of 1 L/min using a compressor. The mixture was then heated using a microwave at varying power levels (300 W, 450 W, and 600 W) until vapor was produced. The vapor was condensed into distillate consisting of two phases: the essential oil as the upper phase and distilled water as the lower phase. The distillate was collected every 20 minutes during the 180-minute extraction process. The results showed that smaller particle sizes and higher microwave power increased the yield of essential oil at an extraction duration of 180 minutes using the MAHD method. The highest essential oil yield from white pepper leaves was 0.4288% (1 cm, 600 W), while the highest yield from seeds was 3.0018% (80 mesh, 600 W). Optimization using RSM–BBD resulted in optimal conditions for leaf oil extraction at a particle size of 1.021 cm, time 179.49 minutes, and microwave power 489.79 W, with a predicted yield of 0.410% and desirability value of 1. For seed oil extraction, the optimum conditions were 88.41 mesh, 180 minutes, and 600 W, with a predicted yield of 2.967% and desirability value of 0.979. The best kinetic model for leaf oil extraction followed the Power’s Law model with R² = 0.9924–0.9965 and RMSD = 0.0180–0.0281, while for seed oil, the Hyperbolic model showed the best fit with R² > 0.999 and RMSD = 0.0053–0.0076. The essential oil from white pepper leaves was green in color, with a relative density of 0.7999, refractive index of 1.4950, and solubility of 1 mL in 10 mL of 95% ethanol. The main chemical components were β-Elemene (4.82%), (trans)-β-Caryophyllene (2.25%), α-Humulene (2.00%), α-Selinene (6.13%), Germacrene-D (0.27%), Isospathulenol (4.21%), and Neointermedeol (4.96%). The essential oil from white pepper seeds was also green, with a relative density of 0.8796, refractive index of 1.4845, and solubility of 1 mL in 4–5 mL of 95% ethanol. The dominant compounds included α-Pinene (3.65%), Δ-3-Carene (22.36%), D-Limonene (15.32%), β-Myrcene (2.54%), Bicyclo[3.1.1]heptane, 6,6-dimethyl-2-methylene-, (1S)- (8.20%), α-Humulene (2.23%), and (trans)-β-Caryophyllene (18.05%). Antibacterial activity testing against Staphylococcus aureus showed that leaf oil produced an inhibition zone of 1.9005 mm on day 1 and 3.5160 mm on day 5, while seed oil produced 3.1791 mm on day 1 and 3.7333 mm on day 5.
| Item Type: | Thesis (Masters) |
|---|---|
| Uncontrolled Keywords: | Biji lada putih, Daun lada, Microwave air hydrodistillation, Minyak atsiri White pepper seeds, Pepper leaves, Microwave air hydrodistillation, Essential oil |
| Subjects: | Q Science > QD Chemistry > QD416 Essences and essential oils. |
| Divisions: | Faculty of Industrial Technology and Systems Engineering (INDSYS) > Chemical Engineering > 24101-(S2) Master Thesis |
| Depositing User: | Siti Syamsiyah |
| Date Deposited: | 01 Aug 2025 09:38 |
| Last Modified: | 01 Aug 2025 09:38 |
| URI: | http://repository.its.ac.id/id/eprint/124786 |
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