Simultaneous Distillation Extraction Research Articles

Supercritical CO2 Extraction of Terpenoids from Indocalamus latifolius Leaves: Optimization, Purification, and Antioxidant Activity.

This study aimed to investigate the efficacy of supercritical CO2 (SC-CO2) extraction in enhancing the extraction rate, purity, and antioxidant activity of Indocalamus latifolius (Keng) McClure (Poaceae) leaf terpenoids (ILLTs). Crude extracts obtained from leaves were subjected to qualitative and quantitative analyses, revealing neophytadiene, phytol, β-sitosterol, β-amyrone, squalene, and friedelin as the primary terpenoid constituents, identified through gas chromatography-mass spectrometry (GC-MS). Compared with steam distillation extraction (SD), simultaneous distillation extraction (SDE), ultra-high pressure-assisted n-hexane extraction (UHPE-Hex), ultra-high pressure-assisted ethanol extraction (UHPE-EtOH), ultrasound-assisted n-hexane extraction (UE-Hex), and ultrasound-assisted ethanol extraction (UE-EtOH), SC-CO2 exhibited a superior ILLT extraction rate, purity, and antioxidant activity. Scanning electron microscopy (SEM) observations of the residues further revealed more severe damage to both the residues and their cell walls after SC-CO2 extraction. Under optimal parameters (4.5 h, 26 MPa, 39 °C, and 20% ethyl alcohol), the ILLT extraction rate with SC-CO2 reached 1.44 ± 0.12 mg/g, which was significantly higher than the rates obtained by the other six methods. The subsequent separation and purification using WelFlash C18-l, BUCHI-C18, and Sephadex LH-20 led to an increase in the purity of the six terpenoid components from 12.91% to 93.34%. Furthermore, the ILLTs demonstrated cytotoxicity against HepG2 cells with an IC50 value of 148.93 ± 9.93 μg/mL. Additionally, with increasing concentrations, the ILLTs exhibited an enhanced cellular antioxidant status, as evidenced by reductions in both reactive oxygen species (ROS) and malondialdehyde (MDA) levels.

Volatile Constituents of Some Myrtaceous Edible and Medicinal Fruits from the Brazilian Amazon.

Native and exotic fruits from the Amazon have varied characteristics, with aroma being a decisive factor in their acceptance for medicinal use as a nutraceutical supplement. This work aimed to analyze the chemical constituents of the volatile concentrates of some Myrtaceous fruit species sampled in the Brazilian Amazon. The fruit's pulps were subjected to simultaneous distillation-extraction, and gas chromatography-mass spectrometry was used to analyze their volatile chemical composition. In the volatile concentrate of Eugenia stipitata (Araçá-boi) α-pinene (17.5%), citronellyl butanoate (15.6%), and pogostol (13.5%) were identified as primary constituents; Eugenia uniflora (Ginja) concentrate comprised curzerene (30.5%), germacrone (15.4%), atractylone (13.1%), and (E)-β-ocimene (11.1%); in Myrciaria dubia (Camu-Camu), α-pinene (55.8%), (E)-β-ocimene (13.1%), and α-terpineol (10.0%) were present; in Psidium guajava (Goiaba) were (2E)-hexenal (21.7%), hexanal (15.4%), caryophylla-4(12),8(13)-dien-5-β-ol (10.5%), caryophyllene oxide (9.2%), and pogostol (8.3%); and in Psidium guineense (Araçá), limonene (25.2%), ethyl butanoate (12.1%), epi-β-bisabolol (9.8%), and α-pinene (9.2%) were the main constituents. The analyzed volatile concentrates of these fruit species presented a significant diversity of constituents with a predominance of functional groups, such as monoterpenes, sesquiterpenes, and fatty acid derivatives, originating from the plant's secondary metabolism and playing an important role in their nutritional and medicinal uses.

Characteristic odor of foxtail millet from different area with different sowing time based on gas chromatography-mass spectrometry

The odor of the foxtail millet is one of the most important indexes to evaluate the foxtail millet quality. Different sowing time results in different quality of the foxtail millet, and the volatiles can be used as fingerprint for distinguish them. The odor components of foxtail millets from spring sowing area and summer sowing area were investigated by means of gas chromatography-mass spectrometry (GC-MS) combined with simultaneous distillation extraction (SDE). A total of 53 volatile compounds were identified in all the samples containing 19 aldehydes, 4 alcohols, 7 ketones, 7 benzene derivatives, 12 hydrocarbons, 3 heterocycles and 1 acid. Aldehydes were the predominant odor components in foxtail millet. Compared with summer sowing area, there were abundant variety and high content of odor components in spring sowing area. Twenty-one volatiles were found to be odor-active compounds. The components with the highest OAVs in most sowing area were (E,E)-2,4-decadienal, (E)-2-nonenal, (E,E)-2,4-nonadienal and nonanal. Finally, 20 volatiles were screened out to distinguish the foxtail millet from spring-sowing area and summer-sowing area by multivariate statistical analysis. The results will be helpful to identify the foxtail millet from different sowing seasons and provide evidence that the spring-sowing foxtail millet shows more active odors.

Unraveling the contributing factors of stale odor in Longjing tea through a sensomics approach

Longjing tea is renowned for its fresh aroma and high value. However, during storage, the emergence of an off-flavor known as “stale odor” can significantly impact the flavor quality and economic benefits of Longjing tea. Yet, the specific volatiles responsible for this stale odor in Longjing tea remain unknown. In this study, Longjing tea samples with varying degrees of stale odor intensity were analyzed using simultaneous distillation extraction coupled with gas chromatography-mass spectrometry (SDE-GC–MS). Through odor activity value (OAV) and fractional omission testing, hexanoic acid and trans-2-nonenal were identified as the primary contributors to the stale odor. Moreover, the concentration of hexanoic acid was found to be valuable in predicting the intensity of the stale odor in Longjing tea. The oxidative degradation of linoleic acid was proved as the generation pathway of stale odor in Longjing tea. These findings provide essential theoretical principles for Longjing tea production and preservation.

Shale primary porosimetry based on 2D nuclear magnetic resonance of T1-T2

Porosity, a key parameter in assessing the physical properties of shale reservoirs and the reserves, is of great significance to the selection and evaluation of shale sweet spots. There are many methods at present to characterize shale porosity, most of which are aimed at post-core cleaning shale, such as those involving helium and saturated fluid (namely liquid-involved porosimetry). However, due to the low efficiency of shale core cleaning and the possible damage to pore structure during the core cleaning process, it's hard to guarantee the accuracy of porosity measurement. In this regard, we resort to the two-dimensional (2D) nuclear magnetic resonance (NMR) technology of T1-T2 in characterizing the primary shale porosity with samples taken from pressure coring in the 4th member of Shahejie Formation (Sha 4 Member) in well Fanxie 184 in the Jiyang Depression. Moreover, comparative experiments of shale porosity measurement by three methods, namely the simultaneous distillation extraction (SDE), helium and fluid measurement, are carried out simultaneously. The results show that the values obtained by SDE, gas and liquid measurement are similar, which are about 0.6 times of 2D NMR porosimetry. Core cleaning efficiency tends to seriously affect the results involving gas and liquid. In addition, the core cleaning treatment is bound to change the shale pore structure, and this is especially true in clay which tends to swell; consequently, porosity results are to be distorted by gas and liquid methods. It is thereby recommended to utilize the 2D NMR technology to characterize the primary total porosity of shale samples without core cleaning. The effective porosity of samples from pressure coring is determined by T2 cutoff value of around 0.3 ms.

Comparison of radiation-induced hydrocarbons formed in three irradiated oilseeds

To investigate the effect of fatty acid composition and irradiation dose on the radiation-induced hydrocarbons, three oilseeds (i.e., peanut, sesame and flaxseed) were selected and irradiated at 2, 4, 6 and 8 kGy. The radiation-induced hydrocarbons were extracted using simultaneous distillation extraction (SDE) and analyzed by gas chromatography-mass spectrometry (GC-MS). The most abundant fatty acid in peanut, sesame and flaxseed oils was oleic, linoleic and linolenic acid, respectively. Nine radiation-induced hydrocarbons including 1,3-bis(1,1-dimethylethyl)benzene and eight products from palmitic, stearic, oleic and linoleic acid were detected in all irradiated samples, even at 2 kGy. Compared to irradiated sesame and flaxseed, irradiated peanut had more radiation-induced hydrocarbons at the same dose. There was a visible difference in radiation-induced hydrocarbon composition among the three oilseeds. The radiolytic hydrocarbons derived from oleic and linoleic acid were predominant for peanut and sesame, while only oleic acid for flaxseed. The fatty acids in flaxseed were more readily cleaved at the alpha-carbon position compared to peanut and sesame. In addition, the concentrations of all detected radiation-induced hydrocarbons in three oilseeds increased linearly with irradiation dose (R2 = 0.957–0.993). The irradiated oilseeds from three different species could be distinguished by hierarchical cluster analysis based on their radiation-induced hydrocarbons.

Identification of aroma‐active components from cultivated agarwood ‘Qi‐Nan’ based on GC‐O‐MS combined with aroma extract dilution analysis

AbstractAgarwood ‘Qi‐Nan’ is commonly regarded as the highest quality agarwood, and has been highly valued for its fragrance. With the increasing amount of cultivated agarwood ‘Qi‐Nan’ in recent years, evaluation of the aroma compounds was drawn attention. Therefore, the volatile compounds in three cultivated ‘Qi‐Nan’ agarwood samples were extracted by simultaneous distillation‐extraction (SDE) and analysed by GC‐O‐MS, combined with aroma extract dilution analysis (AEDA). A total of 70 volatile compounds were identified from three samples, in which sesquiterpenes and aromatics were characterized as key aroma‐active components. Nine compounds were considered as common aroma‐active volatiles in these three essential oils according to their flavour dilution (FD) activity and relative flavour activity (RFA) value, and among them, dihydro‐β‐agarofuran and 4‐methoxy‐benzaldehyde were the most important aroma‐active compounds. Additionally, three ‘Qi‐Nan’ agarwood samples showed different aroma specificity. TD agarwood was characterized by sweet sandalwood odour due to the dominant aroma‐active compound of β‐Santalol. WS agarwood was distinguished by its woody odour because α‐kessyl acetate was its primary aroma. HQ agarwood was featured by woody, spicy and balsamic odour on account of its main aroma compounds of agarospirol and β‐elemene.

Protective effects of Pimpinella diversifolia DC. root essential oil against lipopolysaccharide/D-galactosamine-induced acute liver injury in mice through inhibiting inflammation and reducing oxidative stress

Acute liver injury (ALI) is a life-threatening syndrome with few therapeutic drugs are available. Excessive inflammatory response and imbalance of the antioxidant system are the hallmark of ALI. Therefore, anti-inflammatory and anti-oxidant treatment would be beneficial for ALI. Pimpinella diversifolia DC. is a perennial aromatic herb of the Umbelliferae family. The whole herb has been used as a medicine for thousands of years by the She ethnic minority of China, and is claimed to have beneficial health effects on liver disease. Its roots are rich in essential oil, but there are few reports on its pharmacological study. Therefore, the aim of the current work was to reveal the hepatoprotective effects of P. diversifolia root essential oil (PDREO). PDREO was prepared by a simultaneous distillation–extraction method and characterized by gas chromatography–mass spectroscopy (GC–MS). The potential application of PDREO in detoxification of liver injury was evaluated using a lipopolysaccharide (LPS)- and D-galactosamine (D-GalN)-induced acute liver injury mouse model. The results showed that the major constituents of PDREO were isodaucene (29.97%), 4-methoxy-2-(3-methyloxiranyl)-phenyl isobutyrate (19.53%), geijerene isomer (12.33%), and 2-methyl-4-methoxy-2-(3-methyl-2-oxiranyl) phenyl butyrate (6.88%). Isodaucene was identified in the essential oil of the Pimpinella species for the first time. Pre-treatment with PDREO (50 mg/kg) and (150 mg/kg) can effectively reduce the serum levels of alanine aminotransferase and aspartate aminotransferase, and dramatically alleviate liver edema, hemorrhage, hepatocyte apoptosis, and necrosis, which may be attributed to the significant anti-inflammatory activity (inhibiting the secretion of inflammatory cytokines and chemokines and reducing the infiltration of monocyte-derived macrophages and neutrophils) and the regulatory effects on oxidative stress (upregulating the expression of antioxidant enzymes such as GPX4, SOD1, and CAT) of PDREO. In addition, PDREO (150 mg/kg) can completely block the death of mice induced by LPS/D-GalN, while the survival rate of mice treated with the clinical first-line drug N-acetylcysteine (300 mg/kg) was only 10%. In light of the results obtained, PDREO is a promising natural detoxification agent, with potential applications in the food and pharmaceutical industries.

Comparative analysis of essential oils from two Satureja species; extraction methods, chemical composition, and antimicrobial activities

This study aimed to investigate the antibacterial and antifungal properties of the essential oils extracted from two medicinal plants, Satureja sahendica and Satureja spicigera. Three different methods, including Multi-walled carbon nanotubes (MWCNT) extraction, Clevenger hydrodistillation (Clevenger HD) extraction, and simultaneous distillation-extraction (SDE), were employed to isolate the volatile components of the two species, and then extraction efficiencies were compared. The composition of the essential oils was analyzed using gas chromatography-mass spectrometry (GC-MS). The results revealed that the two plant species contain a significant amount of oxygenated monoterpenes, while sesquiterpenes have a lower percentage. The main compounds of S. sahendica and S. spicigera essential were thymol (10.28–46.83%), carvacrol (7.81–36.88%), terpinolene (5.73–28.53%), ɣ-terpinene (14.76–16.27%), linalool (5.11–14.43%), p-cymene (8.23–12.33%), terpinen-4-0l (4.93–9.97%), germacerene (8.19–9.44%), α-pinene (5.22–8.41%), thymoquinane (4.49–7.65%), 1,8-cineole (4.82–6.83%), spathulenol (3.01–5.47%). To study the antibacterial and antifungal effects of the obtained essential oils, the micro broth dilution method was used on four bacterial species, including Staphylococcus aureus, Escherichia coli, Bacillus subtilis, and Pseudomonas aeruginosa, as well as the fungus Candida albicans. The results indicated that both species essential oils had a high activity against C. albicans, while P. aeruginosa was the most resistant bacteria. Furthermore, it was found that S. sahendica essential oil exhibited a greater antimicrobial effect than S. spicigera. This study provides valuable insights into the antibacterial and antifungal effects of essential oils extracted from S. Sahendica and S. Spicigera, which have potential applications in medicinal industry.

GC-O-MS Analysis of Aroma-Active Compounds of Chinese Almonds Obtained by Different Pretreatment Methods

Almonds (Prunus dulcis) are an ancient and commercially valuable crop from Asia. In this experiment, solid-phase microextraction (SPME), solvent-assisted flavor evaporation (SAFE), and simultaneous distillation extraction (SDE) were used to pretreat the almonds from China. The almond extract was then analyzed by aroma extract dilution analysis (AEDA) with gas chromatography-olfactory-mass spectrometer (GC-O-MS). SPME and SAFE were identified as the better extraction methods, and 52 aroma-active compounds of almonds, such as 1-nonanal, eugenol, and linalool, were identified based on odor activity values (OAVs). Aroma recombination and omission experiments showed that “sweet,” “fruity,” and “fatty” are the main aroma attributes of Chinese almonds, with a strong relationship with hexanal, heptaldehyde, 1-nonanal, etc. This experiment provides new insights into the sensory contribution of Chinese almond volatiles and helps Chinese almond producers characterize and market the aroma profile of Chinese almond varieties.

Chemical Composition, Antitumor Properties, and Mechanism of the Essential Oil from Plagiomnium acutum T. Kop.

Plagiomnium acutum T. Kop. (P. acutum) has been used as a traditional Chinese medicine for thousands of years to treat cancer but lacks evidence. The objective of this work was to reveal the chemical composition of P. acutum essential oil (PEO) and explore its potential antitumor activity and molecular mechanism. PEO was prepared by the simultaneous distillation-extraction method and characterized by gas chromatography/mass spectroscopy. CCK8 assay, flow cytometry, western blot, and immunofluorescence techniques were used to analyze the effects and mechanism of PEO against cancer cells. A total of 74 constituents of PEO were identified, with diterpenes (26.5%), sesquiterpenes (23.89%), and alcohols (21.81%) being the major constituents. Two terpenoids, selina-6-en-4-ol and dolabella-3,7-dien-18-ol, were detected in PEO for the first time. PEO showed significant cell growth inhibitory activity on HepG2 and A549 cells by blocking the G1 phase and inducing apoptosis, which may be attributed to its upregulation of p21Cip1 and p27Kip1 proteins and interference with mitochondrial membrane potential effect. Dolabella-3,7-dien-18-ol accounts for 25.5% of PEO and is one of the main active components of PEO, with IC50 values in HepG2 and A549 cells of (25.820 ± 0.216) µg/mL and (23.597 ± 1.207) μg/mL, respectively. These results confirmed the antitumor medicinal value of P. acutum and showed great application potential in the pharmaceutical industry.

Comparison of Odorants in Beef and Chicken Broth-Focus on Thiazoles and Thiazolines.

The shift in consumer landscape towards vegan, vegetarian and flexitarian diets has created an unprecedented challenge in creating meat aroma from plant-based alternatives. The search for potential vegan solutions has thus led to a renewed interest in authentic meat flavour profiles. To gain a better understanding of the qualitative odour differences between boiled beef and boiled chicken, aroma extracts were isolated using Likens-Nickerson simultaneous distillation-extraction (SDE), selected expressly because the in-situ heating of the sample facilitates the capture of aroma intermediates during the cooking process, thereby mimicking the cooking of meat in stocks and stews. The extracts were then analysed by Gas Chromatography-Mass Spectrometry (GC-MS) and GC-Olfactometry (GC-O). Most of the volatiles identified in this study were sulfur-containing compounds, such as sulfides, thiols, mercaptoaldehydes and mercaptoketones, which are derived from the Maillard reaction. Meanwhile, lipid oxidation results in the formation of unsaturated aldehydes, such as alkenals and alkadienals. Families of thiazoles and 3-thiazolines were found in the extracts. Two novel 3-thiazolines (5-ethyl-2,4-dimethyl-3-thiazoline and 2-ethyl-4,5-dimethyl-3-thiazoline) which may also contribute to the meaty aroma were identified in this work and synthesised from their respective aldehyde and mercaptoketone precursors.

Volatile chemical composition of Octoblepharum albidum Hedw. (Bryophyta) from the Brazilian Amazon

Bryophytes have a variety of bioactive compounds that can be used in biotechnological processes. The objective of this study was to know the volatile chemical composition of Octoblepharum albidum Hedw. from the Amazon and investigate its association with possible bioactive effects on insects. The volatile concentrate of O. albidum was obtained by micro-scale simultaneous distillation–extraction and analyzed by gas chromatography coupled to mass spectrometry and the identification of the compounds was based on system libraries and specialized literature. Twelve organic compounds (92.44% of the total) were identified. Hexadecanoic acid, oleic acid, E-isoeugenol, 1-octen-3-ol, and stearic acid were the major compounds. Most of the compounds have already been reported from bryophytes, while others have an unprecedented occurrence in the group. All identified compounds have biological activities reported in the literature and may participate in plant defense mechanisms against insects, causing mortality or developmental inhibition. In this study, we describe for the first time the volatile chemical composition of O. albidum from Brazil and provide evidence that this species is a source of bioactive compounds. The identified compounds have been reported in the literature to cause mortality or affect the biological parameters of insects, what suggests the possibility of their usage in the formulation of bioinsecticides.

Volatile compounds released by acid hydrolysis in jackfruit (Artocarpus heterophyllus Lam.). A comparative study by using SDE and HS-SPME techniques

The volatile compounds of jackfruit (Artocarpus heterophyllus Lam.) released using acid hydrolysis were comprehensively investigated by using simultaneous distillation-extraction (SDE) and headspace-solid phase microextraction (HS-SPME); both coupled to gas chromatography-mass spectrometry (GC-MS). Hydrolyses were carried out at pH 3 to promote the release of aglycones and pH 7 to inhibit enzymatic reactions. Volatile profiles were analyzed by extraction technique. Besides, the aroma potential (AP) of jackfruit was determined. Sixty-nine volatile compounds were identified. Limonene, pentyl 3-methylbutanoate, 1-butanol, butyl 3-methylbutanoate, butanal, and β-cyclocitral were the prominent compounds. The AP of jackfruit was 3.1 and 3.8 mg/kg by utilizing SDE and HS-SPME respectively. The AP of jackfruit released by acid hydrolysis suggests its use as raw material for foodstuffs prepared under thermal and acid conditions at low pH values, promoting the release of aroma precursors and enhancing the flavor of the final product.

Discovery of flavouring compounds to substitute fatty and tallow characteristics in plant‐based patties

SummaryPlant‐based meat substitutes have greatly improved in recent years in texture and flavour; however, they still lack the authentic fatty and tallow flavour notes associated with meat. To investigate what may be lacking in these products, charred beef was prepared, extracted and analysed in depth, to discover novel high‐impact volatile molecules of sensory value for improved flavour application in plant‐based meat substitutes. Beef was prepared by charring on a grill and extracted by simultaneous distillation extraction (SDE) and solvent‐assisted flavour evaporation (SAFE). The extracts were analysed by gas chromatography–mass spectrometry (GC–MS) and liquid chromatography–mass spectrometry (LC–MS), respectively, which showed the results of 209 volatile compounds and 21 targeted amino acids in the cooked beef. Using GC‐Olfactometry, five compounds were postulated, synthesised and sensorially evaluated to find their optimal use concentrations. Of particular interest were 3‐(methylthio)‐alkanals, some of which had not previously been reported in natural products. A model meat flavour was evaluated with and without 3 of these fatty, tallow compounds at optimal dosage use, when applied to soy and pea protein patties, respectively. Sensory and statistical data analysis showing the resulting organoleptic improvements are also presented.

Unveiling Chemical Cues of Insect-Tree and Insect-Insect Interactions for the Eucalyptus Weevil and Its Egg Parasitoid by Multidimensional Gas Chromatographic Methods.

Multidimensional gas chromatography is, presently, an established and powerful analytical tool, due to higher resolving power than the classical 1D chromatographic approaches. Applied to multiple areas, it allows to isolate, detect and identify a larger number of compounds present in complex matrices, even in trace amounts. Research was conducted to determine which compounds, emitted by host plants of the eucalyptus weevil, Gonipterus platensis, might mediate host selection behavior. The identification of a pheromone blend of G. platensis is presented, revealing to be more attractive to weevils of both sexes, than the individual compounds. The volatile organic compounds (VOCs) were collected by headspace solid phase microextraction (HS-SPME), MonoTrapTM disks, and simultaneous distillation-extraction (SDE). Combining one dimensional (1D) and two-dimensional (2D) chromatographic systems—comprehensive and heart-cut two-dimensional gas chromatography (GC×GC and H/C-MD-GC, respectively) with mass spectrometry (MS) and electroantennographic (EAD) detection, enabled the selection and identification of pertinent semiochemicals which were detected by the insect antennal olfactory system. The behavioral effect of a selected blend of compounds was assessed in a two-arm olfactometer with ten parallel walking chambers, coupled to video tracking and data analysis software. An active blend, composed by cis and trans-verbenol, verbenene, myrtenol and trans-pinocarveol was achieved.

Simultaneous distillation-extraction for manufacturing ultra-high-purity electronic-grade octamethylcyclotetrasiloxane (D4)

Ultra-high-purity (UHP) electronic-grade octamethylcyclotetrasiloxane (D4) is the key precursor of low-dielectric constant (low-k) SiCOH films to manufacture integrated circuits (IC), meeting the stringent requirements of the rapidly developing semiconductor industry. Commonly, metallic impurities in D4 were removed by multiple unit operations of adsorption, filtration, and distillation, which could reduce the concentration of a single metallic impurity below 1 ppb. However, D4 with higher purity is required by semiconductor production due to an increase in transistor density. Herein, a novel method based on the integrated simultaneous distillation–extraction (SDE) was developed for manufacturing UHP electronic-grade D4. The lab and pilot scale experiments showed that the purity of water and D4 has a positive correlation. Based on the experimental data, a double-column process, consisting of azeotropic/extractive distillation column and precision distillation column with UNIQUAC method, was established to access the feasibility of scaling up the SDE process. According to the simulation results, D4 with the purity > 99.999 wt.% and total metallic impurities (TMI) content below 1 ppb could be obtained using ultra-pure water.

Simultaneous Distillation–Extraction of Essential Oils from Rosmarinus officinalis L.

The present study describes a procedure to isolate essential oils from Rosmarinus officinalis L. using simultaneous distillation–extraction (SDE). Rosmarinus officinalis L. can be used for medicinal purposes, as well in the cooking and cosmetics industries. SDE technique extraction combines a steam distillation combined with a continuous extraction using a solvent or a co-solvent mixture, providing faster extractions with low extraction solvent volumes. The effect of the solvent nature and the extraction time on the simultaneous distillation–extraction efficiency was evaluated. The best performance was achieved using pentane as a solvent for 1 h of extraction. The essential oils obtained by simultaneous distillation–extraction extracts were analyzed by gas chromatography with flame ionization detection (GC-FID). Extraction efficiencies ranged from 40 to 70% for the majority of the compounds tested, and the precision (measured by the relative standard deviation) varied between 6 and 35%. Among the compounds analyzed the most abundant in the Rosmarinus officinalis L. sample were 1,8-cineole, (-) –borneol, α-pinene, (S)-(-)- α–terpineol, (-)-bornyl acetate, linalool, and 2,2,6-trimethylcyclohexanone. The SDE method proved to be a suitable option for obtaining extracts free from cuticular waxes or chlorophylls.

Simultaneous Distillation Extraction (SDE) and Headspace Solid-Phase Microextraction (HS-SPME) for the Determination of Volatile Organic Compounds (VOCs) by Gas Chromatography – Mass Spectrometry (GC-MS) in Perilla Frutescens Foliage from South Korea

In the recent past, meat consumption has increased around the world, which resulted in high consumer demand for fresh perilla leaves. The present study aimed at comparison of the volatile organic compounds (VOCs) among three varieties of Perilla frutescens leaves from South Korea via simultaneous distillation extraction (SDE) and headspace solid phase microextraction (HS-SPME). A total of 138 VOCs were identified in leaves of P. frutescens varieties with 111 and 74 VOCs identified by SDE and HS-SPME, respectively. The P. frutescens for. viridis Makino leaves contained the highest concentrations of VOCs for both SDE (17.51 g/kg) and HS-SPME (1.463 g/kg) compared to the other varieties. Perilla ketone was the main volatile in P. frutescens var. acuta Kudo and P. frutescens var. japonica Hara while perilla aldehyde was the major compound in P. frutescens for. viridis Makino. Other major identified compounds were (E)-β-caryophellene, cumaldehyde, limonene, and octanol. Differences in the patterns of functional groups and terpene types were also demonstrated among the varieties. SDE provided more compounds while HS-SPME was more convenient for the determination.

Volatiles Composition and Antimicrobial Activities of Areca Nut Extracts Obtained by Simultaneous Distillation-Extraction and Headspace Solid-Phase Microextraction.

The volatile components of areca nuts were isolated by headspace solid-phase microextraction (HS-SPME, DVB/CAR/PDMS fiber extraction) and simultaneous hydrodistillation–extraction (SHDE) and analyzed by gas chromatography/mass spectrometry. Furthermore, all SHDE fractions were tested for antimicrobial activity using the disk diffusion method on nine Gram-negative and Gram-positive bacteria (Bacillus subtilis, Enterococcus faecalis, Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Streptococcus agalactiae, Streptococcus canis, Streptococcus pyogenes, and Candida albicans). In total, 98 compounds (mainly alcohols, carbonyl compounds, fatty acids, esters, terpenes, terpenoids, and aliphatic hydrocarbons) were identified in SHDE fractions and by using SPME extraction Fatty acids were the main group of volatile constituents detected in all types of extracts. The microorganism most sensitive to the extract of the areca nut was Streptococcus canis. The results can provide essential information for the application of different treatments of areca nuts in the canning industry or as natural antibiotics.