Simultaneous Distillation-solvent Extraction Research Articles

Characterization of odor-active compounds in three varieties of ciruela (Spondias purpurea L.) fruit

ABSTRACTThe aroma-active compounds present in tree ripened fruits of ciruela (Spondias purpurea L.) cultivars Chi abal, Campech abal, and Ek abal were isolated by means of simultaneous distillation solvent extraction and solid-phase microextraction and analyzed by gas chromatography-mass spectrometry. Application of odor activity values (OAV) afforded 22 compounds in higher amounts than their threshold concentrations (OAVs >1). Results of the identification experiments in combination with the OAVs suggested that methyl 3-methylbutanoate, ethyl butanoate, ethyl 2-methylbutanoate, ethyl 3-methylbutanoate, ethyl hexanoate, hexyl acetate, with fruity odor notes; (E)-2-hexenal, (Z)-3-hexen-1-ol, (E)-2-hexen-1-ol, 1-hexanol, and (Z)-3-hexenyl acetate, with grassy odor notes, and limonene (citrus-like) were the potentially important common odorants in all ciruela cultivars. Clear differences in the OAVs of some odorants between each of the cultivars suggested that they contributed to the unique sensory profiles of the individual cultivars.

Effect of Harvest and Drying on Composition of Volatile Profile of Elderflowers (Sambucus nigra) from Wild

Volatile compounds emitted by elderflowers ( Sambucus nigra L.) at various stages (blooming on the bush, and at different stages after harvesting) were analyzed to investigate changes in the composition of volatile profiles induced by two drying procedures. Solid-phase microextraction and simultaneous distillation-solvent extraction were used for concentration of volatiles. Analyses of extracts were performed using gas chromatography coupled with a mass spectrometer or a flame ionization detector. On-site field sampling of volatiles followed-up by chromatographic analysis provided interesting information, including insect pheromones from 55 % to 79 % of the total peak area in the GC/MS chromatograms. Composition of aroma compounds of harvested elderflowers was strongly influenced by the type of drying procedure, where the content of some volatiles decreased and some substances even occur due to ongoing physicochemical processes. Changes in volatile profile caused by harvesting were also observed.

Characterization of aroma-active compounds in choch (Lucuma hypoglauca Standley) fruit

ABSTRACTLucuma hypoglauca Standley, locally named choch, is apparently native from Southern Mexico, but is also cultivated in Central and South America. The fruit is consumed fresh and it is widely accepted in diverse regional markets. Owing to the great potential of commercialization as an exotic fruit, it is important to analyze the aroma of this fruit. The objective of this present study was to analyze the volatile compounds causing the aroma of choch fruit. The volatile compounds of choch fruit were isolated by simultaneous distillation-solvent extraction (SDE) and analyzed by gas chromatography-flame ionization detector and gas chromatography-mass spectrometry. A total of 30 volatile constituents were detected, which represented 2.31 mg kg−1 of the fruit. The composition of the volatile constituents of the fruit included 12 ketones (27.5% of the total volatile composition), seven terpenes (64.8%), four esters (4.1%), four alcohols (2.2%), two aldehydes (1.1%), and a sulfur compound (0.4%). The major compounds were (E)-β-caryophyllene (56.3% of the total volatile composition), with lesser amounts of 3-hydroxy-2-butanone (6.1%), 2-pentanone (5.6%), and (E)-3-penten-2-one (5.6%). By application of odor activity values (OAVs), six constituents were considered as aroma-active volatiles, of which the most important were (E)-3-penten-2-one, (E)-β-caryophyllene, methional, 3-methylbutanal, 3-heptanone, butanal, and 3-hexanone.

Determination of volatile organic compounds, catechins, caffeine and theanine in Jukro tea at three growth stages by chromatographic and spectrometric methods.

Tea contains characteristic volatile organic compounds, polyphenols, caffeine and catechins, and is therefore among the most widely consumed beverages all over the world. In this study, fresh Jukro tea leaves collected from Damyang-gun (Jeollanam-do) at 40, 60 and 90day growth stages, were semi-fermented. The volatile organic compounds (VOCs) were extracted by simultaneous distillation-solvent extraction (SDE) and analyzed by gas chromatography/mass spectrometry (GC/MS). Catechins, caffeine and theanine were analyzed by high performance liquid chromatography (HPLC). A total of 159 VOCs were identified in the analyzed Jukro tea leaves. Comparatively, the increase in the concentrations of VOCs was high in 60day leaves. The content of catechins increased along the three growth stages, whereas caffeine, compared to 90day leaves, was higher for 40 and 60day leaves. Based on the results, the 60day leaves were found to be the most suitable and useful for making semi-fermented Jukro tea.

Comparación entre métodos de extracción para la obtención de volátiles a partir de pulpa de lulo (Solanum quitoense)

Se compararon los métodos de extracción y destilación simultánea (SDE) y microextracción en fase sólida con espacio de cabeza (HS-SPME), acoplados a cromatografía de gases con detector de espectrometría de masas (GC-MS), para la recuperación de volátiles a partir de pulpa de lulo (Solanum quitoense). Se realizó un diseño completamente al azar aplicado al tipo de solvente para SDE/GC-MS, mientras que para HS-SPME/GC-MS se ejecutó un diseño a dos vías, teniendo como factores el tipo de fibra y la temperatura de adsorción. En el primer caso se obtuvieron principalmente hidrocarburos, aldehídos y ésteres; en el segundo, se recuperaron ésteres y aldehídos. El análisis de varianza mostró una interacción significativa entre el tipo de fibra, la temperatura de adsorción y los grupos funcionales.

Volatile Secondary Metabolites from Colombian Croton malambo (Karst) by Different Extraction Methods and Repellent Activity of its Essential Oil

Croton malambo (Karst), is a small tree that grows in the northern Colombian coast and eastern Venezuela. Hydrodistillation (HD), microwave-assisted hydrodistillation (MWHD), simultaneous distillation-solvent extraction (SDE) and supercritical fluid (CO2) extraction (SFE), were employed to isolate volatile secondary metabolites from Colombian C. malambo (Karst) barks. The essential oil and extracts were analyzed by GC-MS. More than 20 individual components in the various extracts were identified. Methyl eugenol was the main component found in the HD and MWHD essential oils (63.5, 74.6 %), SDE and SFE extracts (67.1 and ca. 67.9 %<, respectively), followed by linalool (5.6, 3.4, 4.0 %), trans-β-caryophyllene (2.5, 2.6, 2.1 and 6.5 %) and trans-methyl isoeugenol (1.5, 1.9, 3.2 and 4.2 %). The oil obtained by HD presented a mean lethal concentration (LC50) against Artemia franciscana of 15.32 µg/mL and 2.20 µg/mL after 24 and 48 h exposition, respectively. These results show that C. malambo essential oil is an excellent source of methyl eugenol, but it is moderately cytotoxic. In addition, was evaluated the repellent activity of C. malambo essential oils against an important stored-product insect pest: Tribolium castaneum Herbst. These oils had high repellent effects on T. castaneum (92 % ± 3) at 0.2 µL/cm2 after 4 h of exposure.

Chemical Composition and Antimicrobial and DPPH Scavenging Activity of Essential Oil of Toona sinensis (A. Juss.) Roem from China

The chemical components of essential oil of Toona sinensis leaf blades and their petioles from China were extracted by simultaneous distillation solvent extraction (SDE) and were analyzed by GC-MS. The antimicrobial and DPPH scavenging activity of the essential oil were evaluated. The results showed that there were differences in chemical compositions and content among essential oils extracted from T. sinensis in different parts and different geographical areas in China, but the main components of essential oils were sesquiterpene and sesquiterpene oxygenated compounds, accounting for 90.1% (No. 1), 92.6% (No. 2), and 80.9% (No. 3) of the relative mass fraction, respectively. T. sinensis essential oil exhibited noticeable growth inhibitory activity against the tested microorganisms. The minimal inhibitory concentration (MIC) and minimal bactericidal concentration (MBC) of different essential oils against microorganisms were different. For all essential oil samples, MIC and MBC against Escherichia coli and Bacillus subtilis were less than 25 μg•mL−1, MIC and MBC against Penicillium citrinum were 200 and 400 μg•mL−1, respectively, and MIC and MBC against Colletotrichum gloeosporioides were 50 and 200 μg•mL−1, respectively. The IM50 of DPPH scavenging for T. sinensis essential oil was less than 0.3 g DPPH per g essential oil. The results indicated that T. sinensis essential oil may be a useful natural antiseptic source from forest products.

Characterization of aroma-active compounds in black sapote (Diospyros digynaJacq.)

The volatile compounds of black sapote fruit were isolated by simultaneous distillation-solvent extraction and analysed by gas chromatography-flame ionization detector and gas chromatography-mass spectrometry. A total of 32 volatile constituents were detected, which represented 4.57 mg kg−1 of the fruit. The composition of volatile constituents of the fruit included 9 terpene compounds (49.1% of the total volatile composition), 11 ketones (9%), 5 aldehydes (29.2%), 4 alcohols (3.6%), 2 esters (8.2%) and a paraffin (0.8%). Major compounds were (Z)-b-ocimene (26.6% of the total volatile composition), (E)-cinnamaldehyde (25.5%) and limonene (17.0%). By application of odour activity values, seven constituents were considered as aroma-active volatiles, from which the most important were (E)-cinnamaldehyde, 3-methylbutanal, limonene, (Z)-β-ocimene, linalool, methyl (E)-cinnamate, and β-caryophyllene.

Characterization of aroma-active compounds in sugar apple (Annona squamosaL.)

The volatile compounds of sugar apple fruit were isolated by simultaneous distillation-solvent extraction and analysed by gas chromatography-flame ionization detector and gas chromatography-mass spectrometry. A total of 75 volatile constituents were detected, 53 of them were positively identified. The composition of the fruit included 14 monoterpene hydrocarbons, 17 oxygenated monoterpenes, 14 sesquiterpene hydrocarbons, 11 oxygenated sesquiterpenes, 7 aliphatic esters, 2 aliphatic alcohols, 3 aliphatic carbonyls, 6 aromatics, and a nitrogen compound. Major compounds were α-pinene (24.2%) and β-pinene (20.4%). By application of odour activity values, thirteen constituents were considered as aroma-active volatiles, from which the most important were a-pinene, limonene, myrcene, linalool, and b-pinene.

Volatiles from Syzygium paniculatum Fruit

The volatile compounds of Syzygium paniculatum Banks ex Gaertn. fruit were isolated by simultaneous distillation-solvent extraction and analyzed by gas chromatography-flame ionization detectection and gas chromatography-mass spectrometry. A total of 155 volatile constituents were identified, accounting for 24.5 mg/kg of the fruit composition. Major compounds were alpha-pinene (32.8% of the total composition), (Z)-beta-ocimene (21.8%), limonene (6.9%), and alpha-terpineol (5.1%), indicating that the volatile composition of the fruit is more rich in terpenes.

Scent Composition from Flowers of Allamanda cathartica L. from Cuba

The chemical composition of the volatile oil of Allamanda cathartica obtained by simultaneous distillation-solvent extraction of flowers was analyzed using GC-FID and GC-MS. A total of 42 compounds were identified, from which major components were n-tricosane (17.0 %), 1,8-cineole (12.6 %), n-pentacosane (11.4 %) and (E,E)-geranyl linalool (11.3 %).

Comparisons of Microwave-Assisted Extraction, Simultaneous Distillation-Solvent Extraction, Soxhlet Extraction and Ultrasound Probe for Polycyclic Musks in Sediments: Recovery, Repeatability, Matrix Effects and Bioavailability

The extraction method of pharmaceutical and personal care products (PPCPs) has become a popular issue due to the emergence of PPCPs as contaminants. In this work, polycyclic musks, a typical type of PPCPs, were selected to test various techniques including microwave-assisted extraction (MAE), simultaneous distillation-solvent extraction (SDSE), Soxhlet extraction (SE), and ultrasound probe (UP). MAE and UP proved to be more effective pretreatment techniques than SE and SDSE, with high recovery, repeatability, accuracy, efficiency, little solvent consumption, and acceptable matrix effects. Notably, the chemical methods usually did not work well for the determination of bioavailability and the environmental fate of pollutants was overestimated. In this work, wheat (Triticum aestivum L.) was used as the ecological receptor to evaluate the bioavailability of chemical pollutants. The concentrations of polycyclic musks in sediments by way of UP extraction had a significant correlation (R 2 > 0.9, P < 0.01) with the concentrations in roots of wheat and the changes of chlorophyll, malondialdehyde and peroxidase in leaves of wheat. These changes suggest that the concentrations of polycyclic musks in sediments using UP extraction were comparable with the level of those in vivo. Through this work, it was discovered that using UP with a different solvent was suitable for determining total concentrations and the bioavailable fractions in sediments.

Analysis of Volatile Compounds of Sour Guava (Psidium guineense Swartz) Fruit

Volatile compounds from sour guava (Psidium guineense Swartz) fruit were isolated by headspace solid-phase microextraction (HS-SPME) and simultaneous distillation-solvent extraction (SDE), and identified by GC-FID and GC/MS. A total of 181 compounds were reported for the first time in this fruit, 119 and 163 compounds were identified as headspace volatiles and fruit volatiles, respectively. Ethyl butyrate, ethyl hexanoate, β-caryophyllene and selin-11 -en-4α-ol were the major compounds. Esters (69.5%) and terpenes (60.8%) were the major classes of compounds found in the headspace volatiles and fruit volatiles.

Volatile Compounds of Cassia grandis L. f. Fruit from Cuba

Volatile compounds were isolated from Cassia grandis fruit by simultaneous distillation-solvent extraction. The volatile concentrate was examined by GC and GC/MS. A total of 108 compounds were identified (30.47 mg/kg), from which linalool (31.5% of the total volatiles) was the major compound.

Analysis of Changes in Aroma Components of Pu-erh Tea during Post-fermentation Process

Objective;To reveal the origin of aroma substances in ripe Pu-erh tea and provide guidance for the production of ripe Pu-erh tea by exploring the changes in aroma components during post-fermentation process. Methods;Simultaneous distillation-solvent extraction was applied to extract aroma compounds from Pu-erh tea samples at different post-fermentation stages, and the aroma compounds were analyzed by GC-MS. Besides, these Pu-erh tea samples were subjected to sensory evaluation. Results;65 kinds of aroma components were totally identified in Pu-erh tea samples at different post-fermentation stages, including 11 hydrocarbon kinds, 10 alcohol kinds, 13 aldehyde kinds, 10 ketone kinds, 6 acid kinds, 6 ester kinds, and 9 other compound kinds. The main aroma components of sunshine withering tea were linalool, 4-phenyl-pyridine, phytol, 3,7 dimethyl-1,6- octadiene-3-alcohol, n-palmitic acid, and 4-methyl-2-propyl-1-pentanol, and those of ripe Pu-erh tea were n- palmitic acid, dihydro-kiwi lactone, dihydro lactone anemones, diethyl-2-13 methyl alcohol, and trans-keto- β -malaysia. The relative contents of ketones, aldehydes, acids, and esters increased, but those of alcohols and other compounds decreased over the post-fermentation process. Both type and quantity of methylated substances presented rising trend with the post-fermen- tation extending. The sensory evaluation indicated that the change from clean aroma to stale flavor occurred in the process from sunshine withering tea to ripe Pu-erh tea.

Analysis of Volatile Compounds in Traditional Chinese Fish Sauce (Yu Lu)

Yu lu is a traditional Chinese fish sauce with a strong and distinctive odor. The volatile compounds in the fish sauce made from anchovy (Engraulis japonius) and the snakehead fish (Channa asiatica) were isolated by simultaneous distillation–solvent extraction (SDE) and analyzed by gas chromatography (GC) and mass spectrometry (MS). About 70 volatile compounds were identified, including 20 acids, 4 carbonyls, 14 nitrogen-containing compounds, 14 hydrocarbons, 8 esters, and 3 sulfur-containing compounds. The major contributors to the characteristic odor of the fish sauce are dimethyl disulfide, dimethyl trisulfide, propanoic acid, butanoic acid, 3-(methylthio)-propanol, 2-methylbutenal as well as some nitrogen-containing compounds. Nitrogenous and sulfurous compounds in the fish sauce made from anchovy were more abundant than the fish sauce made from snakehead, while snakehead fish sauce had a greater amount of volatile fatty acids. 3-(Methylthio) propanol could be another important contributor to the distinctive odor of fish sauce.

Composition and Antioxidant Activity of Essential Oils of Lippia Origanoides H.B.K. grown in Colombia

Microwave-assisted hydrodistillation, simultaneous distillation-solvent extraction, and supercritical fluid extraction, were used to isolate secondary metabolites from two Lippia origanoides chemotypes growing wild in Colombia. Compound identification was based on chromatographic and spectroscopic criteria. The main components identified in the essential oil of one chemotype were carvacrol (44.4 – 51.8%) and p-cymene (8.8 – 10.1%). Those of the other chemotype were p-cymene (11.3 – 15.7%) and 1,8-cineole (6.8 – 10.9%). The last one constitutes a new chemotype, characterized by its low thymol and carvacrol contents and very low antioxidant activity. The radical scavenging activity of the essential oil of the first chemotype was higher than that of butylated hydroxytoluene (BHT) and similar to that of α-tocopherol.

Analysis of Volatile Compounds of camu-camu (Myrciaria dubia (HBK) Mcvaugh) Fruit Isolated by Different Methods

Volatile compounds were isolated from camu-camu (Myrciaria dubia (HBK) McVaugh) fruit by liquid-liquid extraction (LLE), simultaneous distillation-solvent extraction (SDE) and headspace solid-phase microextraction (HS-SPME). The volatile concentrates were examined by GC and GC/MS. A total of 111, 114 and 138 compounds were identified in the LLE, SDE and HS-SPME of the fruit, respectively. Limonene was the major component of these concentrates, followed by α-pinene. The relative proportions of the major compounds are shown to be dependent upon the isolation methods.

Rapid Extraction of Volatile Compounds Using a New Simultaneous Microwave Distillation: Solvent Extraction Device

Simultaneous distillation–extraction (SDE) is routinely used by analysts for sample preparation prior to gas chromatography analysis. In this work, a new process design and operation for microwave assisted simultaneous distillation–solvent extraction (MW-SDE) of volatile compounds was developed. Using the proposed method, isolation, extraction and concentration of volatile compounds can be carried out in a single step. To demonstrate its feasibility, MW-SDE was compared with the conventional technique, SDE, for gas chromatography-mass spectrometry (GC-MS) analysis of volatile compounds in a fresh aromatic herb, Zygophyllum album L., a wild salty desert herb belonging to the family Zygophyllaceae. SDE method required a long time (3 h) to isolate the volatile compounds, and large amounts of organic solvent (200 mL of hexane) for further extraction, while MW-SDE needed shorter time (only 30 min) to prepare the sample, and less amount of organic solvent (10 mL of hexane). These results show that MW-SDE–GC-MS is a simple, rapid and solvent-less method for the determination of volatile compounds from aromatic plants.

Constituents of the essential oil of Rhizoma polygonati

AbstractVolatile oil of Rhizoma polygonati (the rhizoma of Polygonatum sibiricum Delar. ex Redoute), was obtained by simultaneous distillation–solvent extraction (SDE). Then the essential oil was analysed by gas chromatography (GC) and gas chromatography–mass spectrometry (GC‐MS). Forty‐two components were identified, constituting approximately 96% of the oil. The main constituents of the essential oil were palmitic acid (50.9%) and ethyl linoleate (28.3%). Copyright © 2006 John Wiley &amp; Sons, Ltd.