Polimerisasi Eugenol Minyak Daun Cengkeh Hasil Redistilasi, Ekstraksi, dan Fraksinasi Menggunakan Katalis Asam Sulfat Pekat

Polymerization of purified eugenol from clove leaf oil using concentrated sulfuric acid as catalyst has been done in this research. Clove leaf oil was purified by vacuum redistillation, acid-base extraction, and vacuum fractionation to yield eugenol. The eugenol was polymerized with concentrated sulfuric acid in ratio 1: 2. Polyeugenol from eugenol of clove leaf oil resulted from redistillation, extraction, and fractionation is in solid form (yield: 88.14%); from redistillation and extraction is also in solid form (yield: 86.15%); from redistillation clove leaf oil is in gel form (yield: 100.29%). Structure of polyeugenol was determined by infrared spectrophotometer and characterized by thin layer chromatography (TLC). Molecular weight of the product was calculated by viscometry method.DOI: http://dx.doi.org/10.15408/jkv.v0i0.468

FRACTIONATION OF FATTY ACID OMEGA 3, 6 AND 9 FROM SNAIL (<i>Achatina fulica</i>) USING COLOUM CHROMATOGRAPHY

The extraction of fat from snail has been carried out by Soxhlet extractor with petroleum ether solvent. Fatty product from extraction was transesterificated in BF3/methanol solvent for an hour by reflux procedure, then extracted by n-hexane to produce methyl ester fatty acid. Free water fatty acid methyl ester was analyzed by Gas Chromatography-Mass spectrometer (GC-MS). Fatty acid ester was separated from its fractions use column chromatography in n-hexane, n-hexane:dietil eter (2:1 v/v), dietil eter, aseton, ethanol and methanol. This fractions wer also analized by GC-MS. From GC-MS data sheet can be obtained 5 fractions which details are; fraction 1 contains omega 3: 27.54 %, omega 6: 15.40 % and omega 9: 6.77 %. Fraction 2 contains omega 3: 3.08 %, omega 6: 15.62 % and omega 9: 10.72 %. Fraction 3 contains omega 6: 3.57 %, omega 9: 7.02 % and none omega 3 inside it. Omega 3, 6 and 9 can't be identification in fraction 4 and 5.   Keywords: extraction, transesterification, column chromatography, GC-M

STUDY OF EPOXIDE DECYCLISATION OF CARYOPHYLENE OXIDE WITH SYNTHETIC ZEOLITE AS CATALYSTS

The reaction of epoxide ring opening of caryophillene oxide has been done using zeolite H-Y, H-sodalit, and H-ZSM-5 as catalysts. The reactions were done in two types, there were in dioxane solvent at temperature of 110 oC and without solvent at temperature of 175 oC. The catalyst weight was 10 % from caryophillene oxide weight, and the time of reaction was four hours. The product of reaction was analyzed using GC, FTIR, and GC-MS. The reactions of caryophillene oxide in dioxane solvent with the three kinds of zeolites did not give any targeted product. Whereas, the reactions without solvent gave three main products, there was one compound with one group of secondary hidroxyl (secondary alcohol), and two compounds of ketone from caryophillene. The reaction product of caryophillene oxide obtained without using solvent with the three type of catalysts were then compared. Conversion of three main products produced by H-ZSM-5 catalyst, H-sodalit catalyst and H-Y catalyst were 82.11 %, 54.92 % and 38.53 % respectively. For that reason, the transformation of caryophillene oxide using H-ZSM-5 catalyst was considered to be the best selective product. The alcohol product was resulted from reaction between caryophillene oxide and Bronsted acid, and  the ketone products was resulted from the reaction with Lewis acid in zeolite.   Keywords: Epoxide ring opening, HY, H-sodalit and HZSM-

Biosynthesis of A6\u277-anhydroerythromycin via enoyl reductase inhibition by isonicotinic hydrazide (INH)

Isonicotinic hydrazide (INH) was added to a fermentation of mutant of Saccharopolyspora erythraea ATCC 11912 to inhibit the activity of 2,4,6,8-tetramethyI-7,9-dihydroxy-2-en-5-on-undecyl-ACP enoyl reductase, an enzyme which catalyses enoyl reduction process of an intermediate in the erythronolide biosynthesis, and produce A"3-anhydroerythromycin derivative. The. optimum INH additional concentration of above 0.1% was able to inhibit the enzyme activity, and produce A6â¢7-anhydroerythromycin derivative as shown by FT-infrared spectrophotometric analysis of the product after its purification using thin layer chromatography. Keywords: Isonicotinic hydrazide (INH) enoyl reductase â d7-anhydroerythromycin â mutant Saccharopolyspor

Structural elucidation of A6\u277-anhydroerythromycin D using H-NMR-spectrometer

1-1-NMR-spectrometric analysis was carried out to samples I and 2 which were isolated respectively from Saccharopolyspora erythraea ATCC 11912 with and without additional isonicotinic hydrzide (INH). The sample I was confirmed as erythromycin D due to the proton appearance of 12-H at 32.3175 (dq) of the macrolactone, and the absence of 3"-niethoxy proton at 3.31 (s) of its neutral sugar. The sample 2 was confirmed as 46\u277-anhydroerythromycin D due to the presence of 7-H(-C=C-) at 35.343 (dq) instead of the methylene proton at C,and the presence of proton 12-Hat 82.318 (dq) of the macrolactone

Isolasi dan Identifikasi Senyawa Terpena Hasil Pirolisis Getah Karet Alam (Hevea Brasiliensis)

Isolation and identification of terpenes obtained from the pyrolisis of natural rubber (Hevea brasiliensis) latex have been conducted. The latex was pyrolized under reduced pressure without any solvent. The pyrolysis products contains water, protein and rubber oil. The rubber oil was separated and identified using GC-MS.The results showed that the rubber oil contained 22 compounds. According to literature review, 12 compounds were identified as terpene, including monoterpene, sesquiterpene and diterpene. Monoterpene compounds were isolimonene, l-limonene, P-felandrene, d-limonene and camphene. The identified sesquitterpenes were 2,4a,8,8-tetramethyl-1,1a,4,4a,5,6,7,8-octahydrocyclopropane [d] naphthalene, P-farnasene, a-amorphene, y-amorphene and bisabolene. The analyzed diterpenes were abietadiene and kaurene. The dominant terpene was d-limonene. The d-limonene was isolated using fractional distillation and had the purity of 96.79%

Isolasi dan Identifikasi Senyawa Terpena Hasil Pirolisis Getah Karet Alam (Hevea brasiliensis)

Isolation and identification of terpenes obtained from the pyrolisis of natural rubber (Hevea brasiliensis) latex have been conducted. The latex was pyrolized under reduced pressure without any solvent. The pyrolysis products contains water, protein and rubber oil. The rubber oil was separated and identified using GC-MS.The results showed that the rubber oil contained 22 compounds. According to literature review, 12 compounds were identified as terpene, including monoterpene, sesquiterpene and diterpene. Monoterpene compounds were isolimonene, l-limonene, P-felandrene, d-limonene and camphene. The identified sesquitterpenes were 2,4a,8,8-tetramethyl-1,1a,4,4a,5,6,7,8-octahydrocyclopropane [d] naphthalene, P-farnasene, a-amorphene, y-amorphene and bisabolene. The analyzed diterpenes were abietadiene and kaurene. The dominant terpene was d-limonene. The d-limonene was isolated using fractional distillation and had the purity of 96.79%

EXTRACTION OF PALM OIL’S FREE FATTY ACIDS BY TRIETHYLAMMINE (TEA) IN POLAR-NONPOLAR MIX-SOLVENT

Palm oil contains unsaturated fatty acids that can be oxidated and can make rancidity of the palm oil. One of the trigliserida degradation products is free fatty acid. The usage of triethylammine (TEA) in the polar-nonpolar mix solvents could enhance the free fatty acids extraction efficiency. Free fatty acids extraction from palm oil was carried out for a minute with solvents ratio: TEA 0,00-0,20M in the following solvent: 0-99% diethyl ether + 99-0% ethanol + 1% water, % volume. The extraction was also performed in the following solvent: TEA 0,00-0,20M in 0-95% heptane + 95-0% isopropanol + 5% water, % volume. Reextraction was conducted for a minute by adding Na2SO4 1M. The alcohol layer which was rich with free fatty acid was taken out and the acid value was determined. As comparison, palm oil's free fatty acids was taken out with standard method by refluxing the sample in 95% alcohol for ten minutes. Identification of the free fatty acids was done by Gas Chromatography-Mass Spectrometer. The best solvent ratio for acid value determination was TEA 0,10-0,20M in the mix-solvent: 19% diethyl ether + 80% ethanol + 1% water, % volume and the extraction product contained 8 kind of free fatty acids. In addition, TEA 0,01M in the solvent: 95% isopropanol + 5% water, % volume could be obtained 8 kind of free fatty acids too. In contrary, the free fatty acid extraction by standard method contained 7 kind of fatty acids. Linoleic acid was the free fatty acid which could not be taken out by standard method. The usage of TEA in the proper polar-non polar mix-solvent was the complete method to determine free fatty acid contained in the palm oil.     Keywords: triethylammine, free fatty acid, organic extraction

Synthesis, antimalarial activity assay and molecular docking study of N-substituted chloro-pyrazolines

Purpose: To synthesize chloro-pyrazolines (A–D), determine their antimalarial activity against Plasmodium falciparum strain 3D7 in vitro, and understand the interaction between falcipain-2 active sites and synthesized compounds by molecular docking simulation.Methods: Chloro-pyrazolines (A–D) were synthesized via cyclo-condensation of 4-chloro chalcone derivatives using several types of hydrazines, i.e., formylhydrazine, benzoylhydrazine, phenylhydrazine and chlorophenylhydrazine. The compounds were analyzed and subjected to antimalarial assay against P. falciparum 3D7. Molecular docking was performed using AutoDock Tools and AutoDock Vina, while each docked compound was visualized using Discovery Studio Visualizer.Results: Pyrazolines A–D yield was 87.09, 61.71, 50.24 and 57.64 %, respectively. Antimalarial assay showed half-maximal inhibitory concentration (IC50) values of 16.46 and 5.55 μM for pyrazoline A and B, respectively, and ≥ 100 μM for pyrazoline C and D. Molecular docking study revealed that pyrazolines A–D had good interaction with the active site of falcipain-2 receptor.Conclusion: A series of N-substituted chloro-pyrazolines has successfully been synthesized with moderate yield. Pyrazoline B has the highest antimalarial activity against P. falciparum 3D7 with IC50 of 5.55 μM. This finding is supported by molecular docking and indicates that the benzoyl substituent increases the antimalarial activity of pyrazoline B. Pyrazoline B has potentials for clinical application as an antimalaria agent