scholarly journals ISOLATION AND IDENTIFICATION OF MAIN AND SIDE PRODUCTS FROM ADDITION REACTION OF CARYOPHYLLENE OXIDE BY FORMIC ACID

2010 ◽  
Vol 2 (3) ◽  
pp. 155-160
Author(s):  
M Muchalal ◽  
Trisulistyaningsih Rahayu

Main and side products from reaction of caryophyllene oxide and formic acid have been isolated using column chromatography with silica gel 60 G as stationary phase and n-hexane : ethyl acetat (9:1, v/v) as mobile phase. The first and second fraction were analyzed using infrared spectrophotometer, gas chromatography, and gas chromatography-mass spectrometer. Caryophyllene formiate as a main product was found in the first fraction. The side product that had been identified were 4,10,10-trimethyl-7-methylenebicyclo[6,2,0]decane-4-carbaldehyde, 2-(9-hydroxy-4,4,8 trimethyltricyclo[6,3,1,01,5]dodecyl)metanoate, clovanediol,4,11,11-trimethyl-8 methylene-3-bicyclo-[7,2,0]-undecen-5-ol,2,5-(6,10,10 imethyltricyclo[7,2,1,01,9]dodecyl)metanedioat, and derivative of caryophylleneformiate.   Keywords: Isolation, identification, caryophyllene oxide

Jurnal Kimia ◽  
2016 ◽  
Author(s):  
Ni Made Dwi Desiyanti ◽  
I Made Dira Swantara ◽  
I Putu Sudiarta

The study of isolation and identification of the active compounds of soursop (Annona muricata L.) leave extract were conducted . The metabolite extraction was conducted using maceration method with 96 % ethanol. The ethanol extract was used to test the mortility of aphid (Myzus persicae S.), with LC50 of 100 ppm. The n-hexane, chloroform, and n-buthanol were used to fractionate the ethanol extract. The mortality test of those three extracts showed the LC50 of 545.12 ppm, 136.26 ppm and 117.73 ppm, respectively. The n-butanol extract was separated using silica gel column chromatography with chloroform: ethanol: water (5:4:1), as the mobile phase. The fractions resulted were FI, FII, FIII, FIV and FV. The mortality test indicated that FII was the best with LC50 of 596.48 ppm. The FII was purified using silica gel column chromatography, resulting three fractions (FII.1, FII.2 and FII.3).  The mortality test of those fractions indicated that FII.2 showed the best result with LC50 of 601.17 ppm. The UV-Vis and IR spectra showed that FII.2 fraction contained flavonoides under the flavonon family.


2017 ◽  
Vol 1 (1) ◽  
pp. 16
Author(s):  
I Made Dira Swantara ◽  
Wiwik Susanah Rita ◽  
Rr Anisa Hernindy

AbstractThis research aims to isolate and phytochemically test of the toxic isolate from ethanol extract of the sponge Hyrtios erecta taken from the waters of Pari Island beach, Thousand Islands (Jakarta). Extraction of the sponges was carried out by 70% ethanol at room temperature. Partition and purification of the compounds were done by column chromatography with the stationary phase of silica gel and the mobile phase of n-hexane-chloroform (2:8). Toxicity screening test was done based on Bhrine Shrimp Lethality Test (BSLT). The compounds of the active isolate were performed by phytochemical test. Based on the results, it was found that the toxic isolate of Hyrtios erecta sponges has anticancer activity with IC50 of 30,497 ppm. The anticancer isolate contained alkaloid, steroid, and polyphenol compounds


2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
D. Penduka ◽  
L. Buwa ◽  
B. Mayekiso ◽  
A. K. Basson ◽  
A. I. Okoh

Partially purified fractions of the n-hexane extract ofGarcinia kolaseeds were obtained through column chromatography and their constituents were identified through the use of gas chromatography coupled to mass spectrometry (GC-MS). Three fractions were obtained by elution with benzene as the mobile phase and silica gel 60 as the stationery phase and these were named Benz1, Benz2, and Benz3 in the order of their elution. The antiListerialactivities of these fractions were assessed through MIC determination and only Benz2 and Benz3 were found to be active with MIC’s ranging from 0.625 to 2.5 mg/mL. The results of the GC-MS analysis showed Benz2 to have 9 compounds whilst Benz3 had 7 compounds, with the major compounds in both fractions being 9,19-Cyclolanost-24-en-3-ol, (3.β.) and 9,19-Cyclolanostan-3-ol,24-methylene-, (3.β.). The Benz2 fraction was found to have mainly indifferent interactions with ampicillin and penicillin G whilst mainly additive interactions were observed with ciprofloxacin. The Benz3 fraction’s interactions were found to be 50% synergistic with penicillin G and 25% synergistic with ciprofloxacin and ampicillin. A commercially available 9,19-Cyclolanost-24-en-3-ol, (3.β.) was found not to exhibit any antiListerialactivities at maximum test concentrations of 5 mg/mL, suggesting that the compound could be acting in synergy with the other compounds in the eluted fractions ofGarcinia kolaseeds.


2007 ◽  
Vol 4 (4) ◽  
pp. 546-549 ◽  
Author(s):  
A. Ashnagar ◽  
N. Gharib Naseri ◽  
H. Haidari Nasab

Anthralin is medically and chemically an important compound which can be found in rhubarb roots. Anthralin and anthralin derivatives have been used as antipsoriatic drugs. In this research, pure anthralin was isolated from the rhubarb roots by maceration and Soxhlet extraction methods in various polar and non-polar solvents. Successive TLC and column chromatography on silica gel with chloroform as the mobile phase afforded two distinct fractions with Rf= 0.54 and 0.61. The1HNMR,13CNMR, IR, UV and MS spectra showed that the fraction with Rf= 0.61 was anthralin. In both methods, methanol was found to be the most suitable solvent for extraction.


2011 ◽  
Vol 117-119 ◽  
pp. 1361-1364
Author(s):  
Yi Jun Zhang ◽  
Cai Xia Dong ◽  
Jun Chen ◽  
Run Qiang Liu

A bifunctional reagent of terephthaloyl chloride was initially adopted as a spacer reagent to prepare the bonded types of chiral stationary phase (CSP) with cellulose derivatives. (3,5-dimethylphenyl)carbamates of cellulose (CDMPC) regioselectively bonded to small pore (3-aminopropyl)silica gel (APS) were prepared with terephthaloyl chloride as a spacer at the 6-position of the primary hydroxyl group on the glucose unit of cellulose. Enantioseparations of five racemic samples are evaluated on the prepared CSP under normal-phase high-performance liquid chromatographic mode with hexane- isopropylalcohol as the mobile phase. The influence of flow rates and mobile phase compositions on the resolution were investigated. The prepared stationary phase was exhibited an effective chiral recognition.


Author(s):  
J. Suleiman ◽  
K. Singh ◽  
A. Y. Bala ◽  
M. T. Muhammad ◽  
M. S. Yakubu

Potential of column purified fractions of Allium cepa bulb against intermediate hosts of urinary schistosomiasis (Bulinus globosus) was conducted in laboratory condition. The fresh bulbs of A. cepa were purchased from Ramin Kura market of Sokoto, identified and authenticated by a taxonomist. The bulbs were sliced into pieces, air dried and powdered. Extracts were obtained using methanol as polar then purified with silica gel as a stationary phase while N-hexane and ethyl acetate (1:1) as the mobile phase. Thirteen fractions each fraction containing 10 ml of the effluent was collected, the collected extracts were left open for evaporation for 48 hours. Ten adult B. globosus were immersed in 3liters of water containing different concentrations of the fraction and each treatment was replicated three times with control in the same condition without treatment, observations were recorded after 24 hours up to 96 hours. The toxicity experiment showed that fractions (F7, F8, F6 and F9) were most toxic fractions, LC50 after 96 hours was 19.371 mg/l. based on findings from this research it can be concluded that, A. Cepa was very potent and can be used for control of B. globosus in order to prevent urinary schistosomiasis infection in endemic areas and drugs industries may use the extracts of these plants for production of molluscicides.


2021 ◽  
Vol 4 (1) ◽  
pp. 41
Author(s):  
Mahfoozurrahman Khan ◽  
Ali Mohammad ◽  
Qasim Ullah ◽  
Faiz Mohammad

This article studies a new green eco-friendly TLC (thin layer chromatography) using silica gel and polyaniline modified silica gel as stationary phase in combination with ethyl acetate (EA), n-butyl acetate (BA) and butane-1-ol (BO) solutions as mobile phase for the comparative study of migration behaviour of organic dyes to identify the most suitable thin layer chromatographic system for the resolution of co-existing dyes. Better separation efficiency was observed by modifying silica gel with polyaniline as compared to pure silica stationary phase. Densitogrpahic presentation of separations achieved on polyaniline modified silica gel Pani@SG-EB1 was also presented. The thin layer chromatographic system comprising of polyaniline modified silica gel Pani@SG-EB1 as stationary phase and n-butyl acetate:DDW, 5:5 as green mobile phase was observed to be the most favourable for the separation of various combinations of three or four-component mixtures of organic dyes viz. methyl thymol blue, tartrazine, carmoisine, rose bengal, amidoblack 10B, bromopyrogallol red and 4-nitrobenzene dizonium tetrafluoroborate. The effect of presence of cations and anions on separation trend was also examined and the limits of detection of the separated organic dyes were estimated. Fourier transform infrared spectroscopy (FTIR), x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron micrograph (TEM) studies were undertaken to characterize silica gel and modified silica gel (stationary phase). The developed method has been successfully applied for the identification of carmoisine in Solvin cold DS syrup and tartrazine in MefastTM syrup.


2018 ◽  
Vol 68 (2) ◽  
pp. 199-210 ◽  
Author(s):  
Loretta Pobłocka-Olech ◽  
Piotr Migas ◽  
Mirosława Krauze-Baranowska

Abstract Flavonoids in the buds of eight Populus species and hybrids were detected and compared with the aid of an optimized TLC method. Separation of 17 flavonoid aglycones belonging to different groups, namely, flavones, flavonols, flavanones and flavanonols, previously described as constituents of poplar buds, was performed on silica gel plates using a hexane/ethyl acetate/formic acid (60:40:1.3, V/V/V) mixture as the mobile phase. Pinocembrin and pinostrobin were found in the majority of analyzed poplar buds. For quantitative analysis of both compounds, two TLC evaluation modes, densitometric and videodensitometric, were compared and the established methods were validated. Concentrations of flavanones in some extracts differed slightly or significantly due to the analyzed plant matrix complexity and the TLC evaluation mode applied. Poplar buds rich in flavanones originated from P. × canadensis ‘Robusta’ (1.82 and 2.23 g per 100 g, resp.) and P. balsamifera (1.17 and 2.24 g per 100 g, resp.).


Author(s):  
Abeer Fauzi Al-Rubaye ◽  
Imad Hadi Hameed ◽  
Mohanad Jawad Kadhim

Chromatography is the term used to describe a separation technique in which a mobile phase carrying a mixture is caused to move in contact with a selectively absorbent stationary phase. It also plays a fundamental role as an analytical technique for quality control and standardization of phyto therapeuticals. Gas Chromatography is used in the separation and analysis of multi component mixtures such as essential oils, hydrocarbons and solvents. Various temperature programs can be used to make the readings more meaningful; for example to differentiate between substances that behave similarly during the GC process. Intrinsically, with the use of the flame ionization detector and the electron capture detector (which have very high sensitivities) gas chromatography can quantitatively determine materials present at very low concentrations. Plants are a rich source of secondary metabolites with interesting biological activities. In general, these secondary metabolites are an important source with a variety of structural arrangements and properties. Gas chromatography - specifically gas-liquid chromatography - involves a sample being vapourised and injected onto the head of the chromatographic column. The sample is transported through the column by the flow of inert, gaseous mobile phase. The column itself contains a liquid stationary phase which is adsorbed onto the surface of an inert solid. The principle of gas chromatography is adsorption and partition. Within the family of chromatography- based methods gas chromatography (GC) is one of the most widely used techniques. GC-MS has become a highly recommended tool for monitoring and tracking organic pollutants in the environment. GC-MS is exclusively used for the analysis of esters, fatty acids, alcohols, aldehydes, terpenes etc. It is the key tool used in sports anti-doping laboratories to test athlete’s urine samples for prohibited performanceenhancing drugs like anabolic steroids. Several GC-MS have left earth for the astro chemistry studies. As a unique and powerful technology the GC-MS provides a rare opportunity to perform the analysis of new compounds for characterization and identification of synthesized or derivatized compound.


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