Aroma Characteristics of Lavender Extract and Essential Oil from Lavandula angustifolia Mill.

Lavender and its products have excellent flavor properties. However, most studies focus on the aroma profiles of lavender essential oil (LEO). The volatiles in lavender extracts (LEs), either in volatile compositions or their odor characteristics, have rarely been reported. In this study, the odor characteristics of LEs and LEO were comprehensively investigated by gas chromatography-mass spectrometry (GC-MS), coupled with sensory evaluation and principal chemical analysis (PCA). In addition, the extraction conditions of lavender extracts from inflorescences of Lavandula angustifolia Mill. were optimized. Under the optimal conditions of extraction, twice with 95% edible ethanol as the solvent, the LEs tended to contain the higher intensity of characteristic floral, herbal and clove-like odors as well as higher scores of overall assessment and higher amounts of linalool, linalool oxides I and II, linalyl acetate, lavandulyl acetate and total volatiles than LEO. PCA analysis showed that there were significant differences on the odor characteristics between LEO and LEs. The LEO, which was produced by steam distillation with a yield of 2.21%, had the lower intensity of floral, clove-like, medicine-like, pine-like and hay notes, a lower score of overall assessment and lower levels of linalool oxides I and II, linalyl acetate, lavandulyl acetate and total volatiles compared with LEs, whereas the relative contents of linalool and camphor in LEO were significantly higher than that in LEs. Furthermore, the earthy, green and watery odors were only found in LEO. Concerning the odor characteristics and volatile compositions, the LEs had better odor properties than LEO. These results provided a theoretical basis for the industrial preparation of lavender-related products.     

Chemical Composition of the Essential Oil of the New Cultivars of Lavandula angustifolia Mill. Bred in Ukraine

Lavender, otherwise known as Lavandula angustifolia Mill., is widely used in landscaping, and its oil is a valuable raw material used in many industries. Therefore, new varieties of this plant are bred. The essential oil composition obtained from fresh flowers of thirteen new Ukrainian cultivars of L. angustifolia were analysed by GC-MS, and eighty-two components were identified. Linalool and linalyl acetate were principal constituents of all of the samples, and ranged from 11.4% to 46.7% and 7.4% to 44.2%, respectively. None of the studied samples fulfilled the requirements of Ph. Eur. and ISO 3515:2002. The main reason was a high content of α-terpineol (0.5–4.5%) and/or terpinene-4-ol (1.2–18.7%). Our results are in line with multiple researchers showing that the studied lavender oils do not comply with the industry standards despite their authenticity. We also investigated the effect of the growth year on the chemical composition of five tested cultivars grown on the same plots and noticed a considerable variability between years. The obtained experimental data did not show a significant inter-year trend for the content changes of the major components. Our results allow us to deeply characterize the new cultivars and evaluate their oil for a possible use in the industry, or to designate them for future selective breeding.     

A multiple hollow fibre liquid-phase microextraction method for the determination of halogenated solvent residues in olive oil

The present paper describes a method based on the extraction of analytes by multiple hollow fibre liquid-phase microextraction and detection by ion-trap mass spectrometry and electron capture detectors after gas chromatographic separation. The limits of detection are in the range of 0.13–0.67 μg kg^?1, five orders of magnitude lower than those reached with the European Commission Official method of analysis, with three orders of magnitude of linear range (from the quantification limits to 400 μg kg^?1 for all the analytes) and recoveries in fortified olive oils in the range of 78–104 %. The main advantages of the analytical method are the absence of sample carryover (due to the disposable nature of the membranes), high enrichment factors in the range of 79–488, high throughput and low cost. The repeatability of the analytical method ranged from 8 to 15 % for all the analytes, showing a good performance.     

Headspace solvent microextraction: a very rapid method for identification of volatile components of Iranian Pimpinella anisum seed

At the present study, a new and rapid headspace solvent microextraction (HSME), for the extraction and pre-concentration of the volatile components of plant sample into a microdrop was applied. The extraction occurred by suspending a microliter drop of the solvent from the tip of a microsyringe to the headspace of a ripen and powdered dry fruit sample (Iranian Pimpinella anisum seed) in a sealed vial for a preset extraction time, then the microdrop was retracted back into the microsyringe and injected directly into a GC injection port. The chemical composition of the HSME extracts were confirmed according to their retention indexes and mass spectra (EI, 70 eV); and quantitative analysis was performed by GC-FID.Parameters such as the nature of the extracting solvent, particle size of the sample, temperatures of the microdrop and sample, volume of sample and the extraction time were studied and optimized, and the method's performance was evaluated. The optimized conditions were: sample particle size, 1 mm; sample volume, 5 ml (in a 15 ml vial); sample temperature, 60 °C; microsyringe needle temperature, 0 °C; and extraction time, 10 min. Finally, accordingly, the percentage of trans-anethole (the major compound of P. anisum) and the relative standard deviation for extraction and determination of trans-anethole (seven-replicated analysis) were determined to be 90% and 3.9%, respectively.     

Solid‐phase microextraction based method for determination of essential oils components in herbal beverages

A method employing the direct immersion solid‐phase microextraction followed by GC‐MS analysis is presented for the determination of essential oils components in herbal tea infusions, i.e. their direct content in the liquid phase. The extraction performances were compared using five different microextraction fibres. Significant parameters affecting sorption process such as sample amount, sorption and desorption time and temperature, stirring speed, pH adjustment and effect of ionic strength were optimised and discussed. By optimising the key parameters, a detection limits (LOD = S/N × 3) for ten target marker compounds were obtained in the range from 5.3 to 48.2 ng/mL with recoveries ranged between 93.03 and 100.50%. Intra‐day and inter‐day repeatability at three concentration levels were found to be 1.1–15.3 and 7.2–15.5% RSD, respectively. Finally, the optimised procedure enabling a rapid and simple analysis of essential oils was applied for the direct determination of these compounds in ten herbal tea infusions.     

A novel vortex-assisted liquid phase microextraction method for parabens in cosmetic oil products using deep eutectic solvent

ABSTRACT

The parabens, which are harmful to our bodies, are primarily utilized as preservatives in medicine, personal care products and cosmetics. A novel, more efficient, fast and cheap vortex-assisted liquid phase microextraction method based on deep eutectic solvents (DESs) was developed for the determination of parabens. The microextraction conditions were optimized using these solvents and the analytical parameters of the method were determined under optimal microextraction conditions. After extraction, the chromatographic separation of parabens was undertaken using high-performance liquid chromatography-UV detection. Experimental parameters, such as DES type, DES volume, dilution solvent volume and vortex extraction time were optimized. DES6 [ChCl-Ethylene glycol (1/2)] was the most suitable DES to work in this study. Detection limits for this method of 0.053 µg mL^?1 for methylparaben, 0.061 µg mL^?1 for ethylparaben, 0.049 µg mL^?1 for propylparaben and 0.052 µg mL^?1 for butylparaben were obtained. Correlation coefficients (R²) for a concentration range of 0.1–100 µg mL^?1 were higher than 0.9992 and relative standard deviation (RSD) values below 2.91% at parabens concentration of 2.5 µg mL^?1 were obtained. The results of spike/recovery values of real samples were greater than 84%. When compared with other methods, the main advantages include lower LOD, short extraction time, rapidity, repeatability and simplicity.     

Supervised principal components: a new method for multivariate spectral analysis

The supervised principal components (SPC) method was proposed by Bair and Tibshirani for statistics regression problems where the number of variables greatly exceeds the number of samples. This case is extremely common in multivariate spectral analysis. The objective of this research is to apply SPC to near‐infrared and Raman spectral calibration. SPC is similar to traditional principal components analysis except that it selects the most significant part of wavelength from the high‐dimensional spectral data, which can reduce the risk of overfitting and the effect of collinearity in modeling according to a semi‐supervised strategy. In this study, four conventional regression methods, including principal component regression, partial least squares regression, ridge regression, and support vector regression, were compared with SPC. Three evaluation criteria, coefficient of determination (R²), external correlation coefficient (Q²), and root mean square error of prediction, were calculated to evaluate the performance of each algorithm on both near‐infrared and Raman datasets. The comparison results illustrated that the SPC model had a desirable ability of regression and prediction. We believe that this method might be an alternative method for multivariate spectral analysis. Copyright © 2013 John Wiley & Sons, Ltd.     

Acorafuran, a new sesquiterpenoid from Acorus calamus essential oil

The structure of acorafuran (6-isopropyl-4-methyl-7,8-dihydro-6H-naphtho[1,8-bc]furan), a new cadalin-type sesquiterpenoid from Acorus calamus essential oil, was established using spectral data (NMR, mass spectrometry). __________ Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 566–568, November–December, 2006.     

Chemical composition and antibacterial activity of Lavandula coronopifolia essential oil against antibiotic-resistant bacteria

The aim of this study was to analyse the composition of the essential oil (EO) of Lavandula coronopifolia from Morocco and to evaluate its in vitro antibacterial activity against antibiotic-resistant bacteria isolated from clinical infections. The antimicrobial activity was assessed by a broth micro-well dilution method using multiresistant clinical isolates of 11 pathogenic bacteria: Klebsiella pneumoniae subsp. pneumoniae, Klebsiella ornithinolytica, Escherichia coli, Enterobacter cloacae, Enterobacter aerogenes, Providencia rettgeri, Citrobacter freundii, Hafnia alvei, Salmonella spp., Acinetobacter baumannii and methicillin-resistant Staphylococcus aureus. The main compounds of the oil were carvacrol (48.9%), E-caryophyllene (10.8%) and caryophyllene oxide (7.7%). The oil showed activity against all tested strains with minimal inhibitory concentration (MIC) values ranging between 1% and 4%. For most of the strains, the MIC value was equivalent to the minimal bactericidal concentration value, indicating a clear bactericidal effect of L. coronopifolia EO.     

Application of solvent microextraction in a single drop for the determination of new antifouling agents in waters

A new, rapid microextraction technique termed solvent microextraction (SME) has been developed for the simultaneous determination of new generation antifouling agents, in water samples. Chlorothalonil, dichlofluanid and Sea nine 211 were employed as model compounds to asses the extraction procedure and were determined by gas chromatography with electron capture detection. Experimental parameters which control the performance of SME, such as selection of solvent, exposure time, agitation, organic drop volume, and salt concentration were optimized. The new method provided good average enrichment factors of >10.7 for all analytes, good precision (RSD < 8.5%) and good linearity (r2 > 0.9880). The limits of detection (LODs) were in the range of 0.00025-0.003 microg/L (S/N = 3). The SME was performed in different type of natural water samples and acceptable recoveries were obtained for the tested analytes. The results demonstrated that SME is a rapid, accurate and effective preparation method and could be successfully performed for the determination of antifouling agents in water samples.     

Headspace solvent microextraction A new method applied to the preconcentration of 2-butoxyethanol from aqueous solutions into a single microdrop

A new procedure and experimental setup for the headspace solvent microextraction of volatile organic materials from aqueous sample solutions is described. The extraction occurs by suspending a 3-μl drop of the solvent from the tip of a microsyringe to the headspace of a stirred aqueous sample solution for a preset extraction time. The temperature of the microdrop and the bulk of sample solution should be kept constant at optimized values. The sample analyses were carried out by gas chromatography. The procedure was successfully applied to the extraction and determination of 2-butoxyethanol from content of some color samples used for painting the outer coverage of some machines such as coolers, refrigerator, cloths machine, etc. Parameters such as extraction time, nature of extraction solvent, size of microdrop, sample volume, stirring rate, ionic strength and pH of sample solution were studied and optimized, and the method performance was evaluated.     

Extraction and separation of zirconium from hafnium using a new solvent microextraction technique

A simple method based on the dispersive liquid?Cliquid microextraction and a solidification of floating organic drop followed by an inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for the extraction and separation of zirconium from hafnium. In this extraction method, an appropriate mixture of acetone (disperser solvent) and 1-undecanol (extraction solvent) was injected rapidly, into the sample solution containing 2.0?mol?L^?1 nitric acid and metal ions in their complex form with cyanex272 and a cloudy solution was formed. After centrifugation, the test tube was cooled by inserting it into an ice bath for 5?min. The solidified 1-undecanol on the top of the solution was transferred into suitable vial and immediately melted, then, 100.0???L of it was dissolved in 100.0???L of 1-propanol and finally, was injected into an ICP-OES by a flow injection system for analysis. Some effective parameters on the extraction and separation of zirconium and hafnium such as type of extraction and disperser solvents and their volumes, type and concentration of ligands, and the type and concentration of acids have been evaluated and optimized. Under the optimum conditions, the selectivity factor of about 13 was obtained.     

A new terpene ketone,a component of the essential oil ofElsholtzia ciliata

A new terpene ketone which has been called dehydroelsholtsia ketone has been isolated from the essential oil ofElsholtzia ciliata (Thumb.) Hyl. The structure of dehydroelsholtzia ketone as 3-methyl-2-(3-methylbut-2-enoyl)furan has been proposed on the basis of a study of its IR, PMR, mass and¹³C spectra and has been confirmed by its conversion into elsholtzia ketone.     

Essential Oil Profile and Yield of Corolla,Calyx, Leaf,and Whole Flowering Top of Cultivated Lavandula angustifolia Mill. (Lamiaceae) from Utah

Lavandula angustifolia Mill. (lavender) is an essential-oil-bearing plant in the Lamiaceae family. Volatile oil produced through the steam distillation of lavender was examined to establish the essential oil yield and aromatic profile from each portion of the plant—namely, the corolla, calyx, leaf, and whole flowering top. The resulting essential oils were analyzed by GC-FID and GC-MS. The different plant parts generally shared similar compounds but in varying relative percentages. Aromatic profiles of the whole flowering top and calyx were similar, with prominent compounds being linalool acetate (34.3%, 32.0%), linalool (26.5%, 32.9%), lavandulyl acetate (5.6%, 4.9%), terpinen-4-ol (5.3%, 7.0%), and (Z)-β-ocimene (4.5%, 5.4%), respectively. Aromatic profiles for the corolla and leaf were unique. Prominent aromatic compounds of the corolla included linalool acetate (18.4%), linalool (10.8%), epi-α-cadinol (10.0%), borneol (7.3%), and lavandulyl acetate (6.3%). Prominent aromatic compounds of the leaf included epi-α-cadinol (19.8%), γ-cadinene (11.0%), borneol (6.0%), caryophyllene oxide (4.9%), and bornyl acetate (4.8%). Complete profiles and essential oil yields of corolla, calyx, leaf, and whole flowering top were established. This study establishes the influence the corolla, calyx, and leaf exert on the aromatic profile of the whole flowering top and provides insight into authentication of lavender essential oil.     

Optimization of an accelerated solvent extraction dispersive liquid–liquid microextraction method for the separation and determination of essential oil from Ligusticum chuanxiong Hort by gas chromatography with mass spectrometry

In this study, an accelerated solvent extraction dispersive liquid–liquid microextraction coupled with gas chromatography and mass spectrometry was established and employed for the extraction, concentration and analysis of essential oil constituents from Ligusticum chuanxiong Hort. Response surface methodology was performed to optimize the key parameters in accelerated solvent extraction on the extraction efficiency, and key parameters in dispersive liquid–liquid microextraction were discussed as well. Two representative constituents in Ligusticum chuanxiong Hort, (Z)‐ligustilide and n‐butylphthalide, were quantitatively analyzed. It was shown that the qualitative result of the accelerated solvent extraction dispersive liquid–liquid microextraction approach was in good agreement with that of hydro‐distillation, whereas the proposed approach took far less extraction time (30 min), consumed less plant material (usually <1 g, 0.01 g for this study) and solvent (<20 mL) than the conventional system. To sum up, the proposed method could be recommended as a new approach in the extraction and analysis of essential oil.     

On-site field sampling and analysis of fragrance from living lavender (Lavandula angustifolia L.) flowers by solid-phase microextraction coupled to gas chromatography and ion-trap mass spectrometry

Solid-phase microextraction coupled to gas chromatography and mass spectrometry has been applied as a simple alternative method for the analysis of essential oil directly from lavender intact flowering spikes and genuine oils. All recognised major oil constituents were detected by this procedure, with results comparable to those given by a conventional method (organic solvent extraction). Distinctive chromatographic profiles were found for various species.     

Exploring natural essential oil components and antibacterial activity of solvent extracts from twelve Perilla frutescens L. Genotypes

Pharmaceutical active ingredients from medicinal plants can be seen as a gateway to drug discovery with the importance of medical and health care. Perilla frutescens has been traditionally used for medicinal and flavoring purposes, thus aromatic compounds and antimicrobial activity of twelve accessions of three solvent extracts (distilled water, methanol and ethyl acetate) of P. frutescens L. Britt grown under open field was studied. RauTiaTo showed relatively high essential oil (EO) content and EO yield, followed by 203P and J1 genotypes. Twenty four monoterpene hydrocarbons, eighteen sesquiterpenes, eight oxygenated compounds—alcohols, five aldehydes, three phenols, other relatively low contents such as four esters and one phenylpropanoid were found. The chief natural constituents of the EO extracted from perilla genotypes were perillaldehyde in (RauTiaTo, J1, 203P, PS1, JTD3, NP606 and 588P), ß-dehydro-elsholtzia ketone in GB, MP3, and PS3 respectively, followed by perilla ketone in PS2 and 465P. Other natural compounds were limonene, ß caryophyllene, (Z,E)-alpha-Farnesene, shisofuran and trans-shisool. Aqueous extract of PS2, 588P and JTD3, as well as antibiotic gentamicin, inhibited more strongly the growth of Klebsiella spp., than other solvent extracts using disc diffusion method. Gentamicin showed a very strong antibacterial activity against Staphylococcus aureus., Streptococcus pneumonia., Klebsiella spp., Shigella spp., Salmonella spp., Escherichia coli with varying degree of inhibition, while another amoxicillin was only active against bacterial infections Streptococcus pneumonia and Escherichia coli. The combination 2 and 3 of herbal preparation showed the antibacterial activity against Streptococcus pneumonia respectively. These results can be helpful for qualitative and quantitative analyses of this herbal drug and food additives in quality control for the standardisation of natural products.     

Identification and quantification of the antimicrobial components of a citrus essential oil vapor

The anti-bacterial components of a citrus essential oil vapor were identified as linalool, citral and beta-pinene using a bioautography method and quantified by GC-MS. Essential oil vapor release, monitored in real-time with Atmospheric Pressure Chemical Ionization - MS (APCI-MS), showed differences in the vapor release profile oflimonene, beta-pinene and linalool over 24 hours, while Solid Phase Micro-extraction (SPME) GC-MS demonstrated changes in composition of the vapor at 35 degrees C. Fourteen isolates were tested in vitro for their susceptibility to the EO vapor and to linalool, citral and beta-pinene vapors, both separately and in a mixture containing the three components in the amounts at which they occur in the EO vapor. All eleven Gram-positive strains tested were susceptible to the EO vapor, linalool, citral and beta-pinene vapors separately and the mixture with zones of inhibition of 4.34 cm, 5.32 cm, 5.58 cm, 4.86 cm and 4.68 cm, respectively. Of the three Gram-negative strains tested, Pseudomonas aeruginosa 10145 was resistant to all the vapors. When bacteria inoculated onto stainless steel surfaces were exposed to either the EO vapor or a linalool/citral/beta-pinene vapor mixture there was no significant difference in reduction for the Gram-positive isolates, while the Gram-negative isolates were resistant to both EO vapor and the linalool/citral/beta-pinene mixture.     

Comparative Evaluation of the Essential Oil of the New Ukrainian Lavandula angustifolia and Lavandula x intermedia Cultivars Grown on the Same Plots

New cultivars of lavender adapted to arid steppe conditions were developed by the Institute of Rice of Ukrainian National Academy of Agrarian Sciences (NAAS). This work is a part of the characterization process of the new cultivars. The chemical composition of the essential oil of the seven new Lavandula angustifolia and eight new Lavandula x intermedia cultivars was investigated and compared. In total, 71 different compounds were identified. Linalool and linalool acetate were the main components in both species in ranges of 26.14–57.07% and 9.08–24.45%, respectively. They were followed by terpinen-4-ol (2.16–22.44%), lavandulyl acetate (2.12–10.23%), and lavandulol (1.30–3.14) in the case of L. angustifolia and camphor (10.11–12.55%), borneol (5.49–8.71%), and eucalyptol (0.47–7.41%) in the case of L. x intermedia. The oils had a valuable terpene profile—a high linalool content and the substantial presence of lavandulol and its ester. Nevertheless, they did not comply with the industry standards, mostly due to high levels of terpinene-4-ol. Evidently, a high content of terpinen-4-ol is a characteristic feature of L. angustifolia oils bred in Ukraine. Additionally, the LA3 cultivar yielded an oil with some of the highest linalool contents reported in the literature. Statistical analysis and literature data allowed for the comparative analysis of the gathered data. MANOVA, PCA, and HCA marked caryophyllene oxide as another potential differentiating compound between studied species.