Static Headspace Solid-phase Microextraction Research Articles

Efficient Capture of Cannabis Terpenes in Olive Oil during Microwave-Assisted Cannabinoid Decarboxylation.

The development of selective extraction protocols for Cannabis-inflorescence constituents is still a significant challenge. The characteristic Cannabis fragrance can be mainly ascribed to monoterpenes, sesquiterpenes and oxygenated terpenoids. This work investigates the entrapment of Cannabis terpenes in olive oil from inflorescences via stripping under mild vacuum during the rapid microwave-assisted decarboxylation of cannabinoids (MW, 120 °C, 30 min) and after subsequent extraction of cannabinoids (60 and 100 °C). The profiles of the volatiles collected in the oil samples before and after the extraction step were evaluated using static headspace solid-phase microextraction (HS-SPME), followed by gas chromatography coupled to mass spectrometry (GC-MS). Between the three fractions obtained, the first shows the highest volatile content (~37,400 mg/kg oil), with α-pinene, β-pinene, β-myrcene, limonene and trans-β-caryophyllene as the main components. The MW-assisted extraction at 60 and 100 °C of inflorescences using the collected oil fractions allowed an increase of 70% and 86% of total terpene content, respectively. Considering the initial terpene amount of 91,324.7 ± 2774.4 mg/kg dry inflorescences, the percentage of recovery after decarboxylation was close to 58% (mainly monoterpenes), while it reached nearly 100% (including sesquiterpenes) after extraction. The selective and efficient extraction of volatile compounds, while avoiding direct contact between the matrix and extraction solvents, paves the way for specific applications in various aromatic plants. In this context, aromatized extracts can be employed to create innovative Cannabis-based products within the hemp processing industry, as well as in perfumery, cosmetics, dietary supplements, food, and the pharmaceutical industry.

Identifying foliar volatile organic compounds of Plectranthus and Coleus (Lamiaceae) as predictive markers of genus using GC×GC-TOFMS and machine learning

Two prominent plant genera, Plectranthus, and Coleus, many species of which are indigenous to southern Africa, have been previously classified as a single genus of the name Plectranthus. However, phylogenetic analysis of markers of the plastid genome of subtribe Plectranthinae (family: Lamiaceae) has led to the recognition of Coleus as a sister taxon to Plectranthus. The purpose of this study is to analyse the profiles of foliar volatile organic compounds (VOCs), from the leaves of southern African species of Plectranthus and Coleus, as predictive chemotaxonomic markers of genus, using two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) and machine learning. Foliar VOCs from fresh crushed leaves of representative species of each genera (nine Plectranthus, six Coleus) were extracted in triplicate using static headspace solid-phase microextraction (HS-SPME), and analysed using GC×GC-TOFMS. Profiles of the foliar VOCs for each sample were constructed from their total ion chromatograms, and machine learning algorithms were used to model the data, to make predictions on the genus of new samples, and to tentatively identify putative markers of genus for Plectranthus and Coleus. A high predictive accuracy (up to 90%) was obtained, with a sensitivity (for genus Coleus) of up to 100%. Top ranking variables included C6C15 compounds of various chemical classes, but most notably of the sesquiterpene isomers, which were found to occur more prevalently in genus Coleus.

The Application of Essential Oil Vapors at the End of Vacuum Cooling of Fresh Culinary Herbs Promotes Aromatic Recovery.

Aroma is an important quality parameter of fresh culinary herbs that may be highly affected after postharvest treatments. The innovative technology of vapor essential oil (EO) application under vacuum conditions may recover aroma lost during the postharvest processing of plant products like aromatic herbs. Hence, this study assessed the aroma recovery effect of vapor EOs applied during vacuum cooling on curly parsley and dill. The volatile organic compounds (VOCs) profiles of these aromatic herbs were studied by static headspace solid-phase microextraction (SPME), and the VOCs sorption kinetics onto the SPME stir-bar coating were modeled by the Baranyi model. At the pilot plant scale, the total VOCs contents of parsley and dill (whose extractability was increased by 10–20% after a single vacuum process) were enhanced by 4.5- and 2-fold, respectively, when vapor EOs were applied. In particular, 1,3,8-p-menthatriene and carvone (parsley) increased by 18.7- and 7.3-fold, respectively, while dill ether (the characteristic VOC of dill) augmented by 2.4-fold after vapor EOs were applied under vacuum conditions. The aroma recovery of culinary herbs was successfully validated at an industrial level in an installation developed by our group to apply vapor EOs within a vacuum cooling system, reaching total VOC recoveries of 4.9- and 2.3-fold in parsley and dill, respectively.

Floral scent compounds and emission patterns of three Styrax species

Styrax is a gorgeous species combined with high medicinal and ornamental values, however, information about its floral scents is limited. This study aimed to reveal the floral scent compounds and the dynamic changes in the flowering process of Styrax japonicus, S. grandiflora and S. calvescens. Static headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry was adopted in the present study. The results showed that 24, 22 and 22 volatile compounds were present at three flowering stages, among which linalool, ocimene, α-pinene and germacrene D dominated in different species. Terpenes were the main floral scent compounds in all species, whereas there was considerable relative content of ketones in S. japonicus. Among the major terpenes, α-pinene, ocimene and myrcene were the common volatiles in these species, while β-elemene and allo-ocimene were the specific volatiles in S. japonicus and S. calvescens, respectively. The highest content of terpenes occurred at initial flowering stage in three species. The differences in the type and content of principal compounds contributed to the fragrance diversity among these species. A solid foundation for understanding the complexity of volatile emission could be obtained from our findings, meanwhile, effective utilization of abundant terpenes in flowers of Styrax species should be applied.

Profile of Terpenoid Compounds Mediating a Plant-Herbivore Interaction: Screening by Static Headspace Solid-Phase Microextraction-Gas Chromatography/Q-ToF Mass Spectrometry.

Conotrachelus dimidiatus (Coleoptera: Curculionidae) interacts with immature guava fruits (Psidium guajava L.) for feed, sleep, mate and oviposit. Determination of the volatile organic compounds (VOCs) emitted by the insect and immature fruits can help improve understanding of plant-insect and intraspecific insect interactions between females and males of C. dimidiatus. Daytime fruit setting emissions of immature guava consist mainly of limonene, caryophyllene, and aromadendrene. In addition to the host's volatiles, the aim of this study was to assess the VOCs released by the insect. Static headspace-solid phase microextraction (SHS-SPME), combined with gas chromatography/quadrupole time of flight mass spectrometry (GC/Q-ToF-MS), allowed the identification of the C10 terpenoids: grandlure I, II, II, IV, grandisoic acid, papayanol and papayanal bioactive compounds released by female and male C. dimidiatus under laboratory conditions. These chemical compounds are candidates for the preparation of a lure formulation.

Attraction of Adults of Cyclocephala lunulata and Cyclocephala barrerai (Coleoptera: Scarabaeoidea: Melolonthidae) towards Bacteria Volatiles Isolated from Their Genital Chambers.

In the study of the chemical communication of adults of the Melolonthidae family, bacteria have been observed in the epithelium of the genital chamber; possibly, bacteria are involved in the production of sex attractants in their hosts. Therefore, it is important to identify the volatile organic compounds from bacteria (VOCsB) released by these microorganisms and study the biological activity stimulated by VOBCs in adults of Melolonthidae. In this study, bacteria were isolated from the genital chamber of Cyclocephala lunulata and Cyclocephala barrerai, from which VOCsB were extracted using static headspace solid-phase microextraction (SHS-SPME) and dynamic headspace Super Q solid-phase extraction (DHS-SPE) and analyzed using gas chromatography-mass spectrometry. The effect of VOCsB on the hosts and conspecifics was evaluated utilizing an olfactometer and electroantennography (EAG). Two species of Enterobacteria were isolated from the genital chamber of each female species, and VOCsB derived from sulfur-containing compounds, alcohols, esters, and fatty acids were identified. An attraction response was observed in olfactometry studies, and antennal responses to VOCsB were confirmed in EAG bioassays. With these results, new perspectives on the relationship between these beetles and their bacteria emerge, in addition to establishing a basis for management programs in the future.

A chemometric approach to characterize the aroma of selected brown and red edible seaweeds / extracts.

Information pertaining to the aromatic profile of seaweeds and seaweed extracts can provide evidence regarding their potential suitability as ingredients in processed foods. To date only limited material has been available on the volatile profiles of some seaweed species. Others in this study have not previously been described. The volatile profiles of dried brown (Himanthalia elongata, Undaria pinnatifida, Alaria esculenta) and red (Porphyra umbilicalis, Palmaria palmata) seaweeds, and a brown seaweed extract (fucoxanthin) from Laminaria japonica were investigated using a chemometric approach to collate data from volatile gas chromatography - mass spectrometry (GC-MS), direct sensory aroma evaluation, and gas-chromatography - olfactometry (GC-O) to obtain a better understanding of their volatile profile and sensory perception. More than 100 volatile compounds were identified by static headspace solid phase micro-extraction (HS-SPME) and thermal desorption gas chromatography - mass spectrometry (TD GC-MS). Brown seaweeds were characterized by 'grassy/herbal/floral', 'fruity', and 'fatty' aromas, red seaweeds by 'green/vegetable', 'mushroom/earthy' and 'sweet/buttery' aromas, and the fucoxanthin extract by 'rancid' and 'nutty' aromas with an overall lower intensity. Heptanal appeared to be a major odor-active compound in all samples. Other volatiles were more characteristic of each individual seaweed: hexanal, (E,Z)-2,6-nonadienal and 2-pentylfuran for H. elongata; ethyl butanoate and 2,3-butanedione for U. pinnatifida; 6-dimethylpyrazine, (E,Z)-2,6-nonadienal and sulactone for P. palmata; 1-octen-3-ol for P. umbilicalis, heptanone for A. esculenta, and 2-furanmethanol for fucoxanthin. Brown and red seaweeds had distinct sensory properties with individual seaweeds having differing volatiles and odorants. This study provides additional information that can contribute to the development of products incorporating dried seaweeds / extracts that are more acceptable to the consumer. © 2020 Society of Chemical Industry.

Methanethiol, an Off-Flavor Produced from the Thermal Treatment of Mandarin Juices: A Study of Citrus Sulfur Volatiles.

The off-flavor produced after thermal stabilization of mandarin (Citrus reticulata, Blanco) juices has limited the production of commercial juices. Methanethiol, a putrid-smelling sulfur volatile, has been identified for the first time in heated mandarin juices. Identification was achieved using a combination of capillary gas chromatography with two dissimilar columns and a dual sulfur-specific pulsed flame photometric detector and selected ion mass spectrometry detection. Static headspace solid-phase microextraction quantitation found that average odor activity values (OAVs) in heated juices were 25.5 for methanethiol compared to 10.8 for dimethyl sulfide. OAVs for methanethiol and dimethyl sulfide in fresh juices were ND (not detected) and 5.5, respectively. Hydrogen sulfide, carbonyl sulfide, carbon disulfide, and dimethyl disulfide were also identified and quantitated. Thermal decomposition studies of nonvolatile sulfur-containing potential precursors indicated that methionine was the major source of methanethiol. Additional heating studies with model juices demonstrated that ascorbic acid greatly accelerated the formation of methanethiol and methional, as well as dimethyl di and tri sulfides.

Flowering Stage and Daytime Affect Scent Emission of Malus ioensis "Prairie Rose".

Flowering crabapple is an important ornamental flower. It is vital to understand the floral scent properties and the associated release dynamics for carrying out fragrant flower breeding or floral regulation of crabapple. Static headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry was used to detect the volatile compounds in Malus ioensis “Prairie Rose” flowers at different flowering stages and at different day-night time. The results showed that methylheptenone, phenylethanol, geranylacetone, 2-(4-methoxyphenyl)ethanol, α-cedrene were the major compounds in M. ioensis “Prairie Rose”, but the compounds released during different stages and different day-night time were significantly different (P < 0.0001). A total of 25 volatile compounds were identified from the four flowering stages. The floral scents in the initial and flowering stages were the most similar (dissimilarity 0.21). The main compounds in these two stages were geranylacetone and methylheptenone, and the contents of geranylacetone and phenylethanol were positively correlated with the flowering stages. From the bud stage to the end of flowering, the total amount of volatile compounds released showed an initial increase followed by a decrease and the amounts of compounds released during the initial flowering stage were the highest. The aliphatic and benzenoids content was significant higher in the daytime than at night. A total of 15 compounds were detected in the five time periods. Methylheptenone and phenylethanol were particularly released in the 10:00–12:00 and 15:00–17:00 time periods. There were only three common compounds among the five time periods and the types of flower volatiles released during the daytime were obviously higher than those released at night. From the nocturnal to diurnal, the amount of flower volatiles released first increased, then decreased, and the release reached a peak between 10 am and 12 noon, which was consistent with the pollination biological characteristics of Malus flowers. Our findings are important for understanding the mechanism of insect visits to crabapple and the regulation of crabapple flower scent.

Determining the Henry’s volatility coefficient of nitrosamines in CO2 capture solvents

Fundamental properties of nitrosamines, such as their Henry’s law constants, are needed to accurately predict the gas-phase partitioning and mitigate emissions of these volatile compounds from operating CO2 capture systems. In this work, the Henry’s volatility coefficient of several environmentally relevant nitrosamines were experimentally obtained from water, from a concentrated amine solution and from a CO2 loaded amine solution using a static headspace solid phase microextraction and gas chromatography mass spectrometry method. The dimensionless Henry’s volatility coefficients of N-nitrosodimethylamine and N-nitrosodiethylamine were found to be range of 0.001–0.1 at CO2 absorber exit temperatures from 25 to 55 °C. A linear temperature dependency of the Henry’s volatility coefficient for these nitrosamines was observed. CO2 loading in the amine solvent increases the Henry’s volatility coefficient of the more non-polar nitrosamine while it decreased the Henry’s volatility coefficient of the more polar nitrosamine. Similar to parent amines, the polarity of the individual nitrosamines plays a key role in its Henry’s volatility coefficients and gas phase partitioning from concentrated amine solutions.

Aroma volatiles obtained at harvest by HS-SPME/GC-MS and INDEX/MS-E-nose fingerprint discriminate climacteric behaviour in melon fruit.

Melon aroma volatiles were extracted at harvest from juice of a climacteric near-isogenic line (NIL) SC3-5-1 with two quantitative trait loci (QTLs) introgressed which produced climacteric behaviour and its non-climacteric parental (PS) using two methodologies of analysis: static headspace solid phase micro-extraction (HS-SPME) by gas chromatography-mass spectrometry (GC-MS) and inside needle dynamic extraction (INDEX) by MS-based electronic nose (MS-E-nose). Of the 137 volatiles compounds identified, most were found at significantly higher concentrations in SC3-5-1 than in PS in both seasons. These volatiles were mostly esters, alcohols, sulfur-derived esters and even some aldehydes and others. The number of variables with high correlation values was reduced by using correlation network analysis. Partial least squares-discriminant analysis (PLS-DA) achieved the correct classification of PS and SC3-5-1. The ions m/z 74, 91, 104, 105, 106 and 108, mainly volatile derivatives precursor phenylalanine, were the most discriminant in SC3-5-1 and PS. As many as 104 QTLs were mapped in season 1 and at least 78 QTLs in each season with an effect above the PS mean. GC-MS gave better discrimination than E-nose. Most of the QTLs that mapped in both seasons enhanced aroma volatiles associated with climacteric behaviour.

Flavor chemistry of lemon-lime carbonated beverages.

The most potent aroma-active components of Sprite (SP), Sierra Mist (SM), and 7UP (7UP) were identified. Aroma extracts were prepared by liquid–liquid continuous extraction/solvent-assisted flavor evaporation (LLCE/SAFE). Twenty-eight compounds were detected by gas chromatography–olfactometry (GC-O) with linalool (floral, lavender), octanal (pungent orange), and 2,3-dehydro-1,8-cineole (minty) determined to be predominant aroma compounds based on their high flavor dilution (FD) factors by aroma extract dilution analysis (AEDA). The data indicate that lemon-lime flavor is composed of a small number of compounds (22 at the most in SM), and only a subset of these may be important because many compounds were detected only at low FD factors. Predominant aroma compounds (23) were quantified using static headspace solid phase microextraction (SPME) combined with stable isotope dilution assays (SIDA). In contrast to FD factors, the calculated odor-activity values (OAVs) indicate that octanal and limonene make the greatest contribution to the overall aroma of lemon-lime carbonated beverages, followed by nonanal, decanal, linalool, 1,8-cineole, and geranyl acetate. The results demonstrate that lemon-lime carbonated beverages share many of the same compounds but the relative abundance of these compounds varies by brand.

GC–MS study of compounds isolated from Coffea arabica flowers by different extraction techniques

Headspace (HS), extractive, and distillative methods were employed to isolate volatile and semivolatile compounds from fresh Coffea arabica flowers. Static HS solid-phase microextraction (HS-SPME), microwave-assisted HS-SPME (MW-HS-SPME) with simultaneous hydrodistillation, and extraction with hexane or supercritical CO2 -isolated mixtures in which around 150 different chemical substances were identified or tentatively identified by GC-MS analysis. n-Pentadecane (20-37% relative peak area, RPA) was the most abundant compound in the HS fractions from fresh flowers, followed by 8-heptadecene (8-20% RPA) and geraniol (6-14% RPA). Hydrocarbons (mostly C13 -C30 paraffins) were the predominant compound class in all the sorptive extractions (HS-SPME, MW-HS-SPME, distillate), followed by terpenoids or oxygenated compounds (which varied with the isolation technique). Caffeine, a distinctive component of coffee fruits and beans, was also found in relatively high amounts in the supercritical CO2 extract of C. arabica flowers.

Dynamics of the Headspace Chemical Components of Rosa damascena Mill. Flowers Ana Dobreva

It was monitored the daily dynamics of components in the natural essential oil of Rosa damascena Mill. flowers using static headspace solid phase microextraction technique (sHS-SPME). 37 compounds were identified. It was established that the headspace model was a combination of terpene alcohols: geraniol (0.57 - 32.33 %), citronellol (1.18 - 30.93 %), nerol (0.39 - 8.58 %), menthone (1.46 - 20.20 %) and phenylethyl alcohol (1.32 - 13.36 %), whose presence was highly dependent on day moment and abiotic factors (air temperature, relative humidity, intensity of sunlight and wind) at the relevant time.

Aroma Profile Discrimination of Coffees and Industrial Blends According to the Chromatic Value

In the present work, static headspace solid phase microextraction using carboxen/polydimethylsiloxane polymeric fibre (HS-SPME(CAR/PDMS)) followed by gas chromatography-mass spectrometry (GC-MS), revealed the best analytical performance to characterize the aroma profile of coffees and industrial blends with different chromatic values (64.9, 70.6, 75.3, 86.1 and 89.6). The most relevant classes of aroma compounds founded were pyrroles, ketones, pyrazines, furans, phenolics, pyridines, alcohols and acids, independently of the roasting degree. By combining the analytical methodology with principal component analysis (HS-SPME(CAR/PDMS)/GC-MS/PCA), important aroma compounds such as 2-furancarboxaldehyde, 2-furanmethanol and acetic acid, allows to discriminate the different roasting degrees, from light (chromatic value 89.6) to dark (chromatic value 64.9) roast. The proposed analytical approach may help to build aroma profile databases to a better evaluation of coffee blends quality, and in controlling the industrial roasting processes.

Study on Determination Method of the Volatile Organic Compounds Emissions from Particleboards for Indoor Finishing

In order to comprehensive understand and control volatile organic compounds (VOCs) release from particleboards, this paper takes Larix gmelini particleboard as example and analyzes VOCs by three different methods. First of all, VOCs of Larix gmelini particles were detected by the static head space solid-phase micro-extraction (HS-SPME) technique. Secondly Larix gmelini particleboards were analyzed using the method of adsorbed by activated carbon, desorpted with methylene dichloride and measured by GC/MS. Finally, Tenax-T Thermal desorption -GC/MS was used to qualitative VOCs emissions. The best method for determination VOCs from particleboards was found. SPME is a simple operation method with short time. But the pretreatment of sample was troublesome and it is not easily measured for lower concentration particleboards. Active carbon absorption method is not suitable for quantitative because of much error in extraction. It is suitable for qualitative analysis. Tenax-T is a simple operation way with short analysis time and good shape of chromatographic. It is a convenient and practical method. Further study of VOCs emission of panels can be supported by this method.

Identification of New Strawberry Sulfur Volatiles and Changes during Maturation

Two Florida strawberry cultivars, 'Strawberry Festival' and 'Florida Radiance', were harvested at five fruit developmental stages (white, half red, three-quarter red, full ripe, and overripe) at four harvest dates. A static headspace solid-phase microextraction (SPME) sampling technique coupled with gas chromatography (GC) using pulsed flame photometric detection (PFPD) was employed to measure 16 sulfur volatiles in these strawberries. A total of 7 sulfur volatiles have been previously reported, and 9 are reported for the first time in strawberries. Newly identified sulfur volatiles include methyl thiopropionate, ethyl thiobutanoate, methyl thiohexanoate, methyl (methylthio)acetate, ethyl (methylthio)acetate, methyl 2-(methylthio)butyrate, methyl 3-(methylthio)propionate, ethyl 3-(methylthio)propionate, and methyl thiooctanoate. Identifications were based on matching sulfur peak linear retention indexes (LRIs) of unknowns with authentic standards and gas chromatography-mass spectrometry (GC-MS) data. Concentrations were determined using both internal and external standards. Most sulfur volatiles increased with increasing maturity, with only concentrations of hydrogen sulfide and methanethiol remaining relatively consistent at all five stages. At the white and half red stages, most sulfur volatiles consisted of various alkyl sulfides. At three-quarter red (commercial ripe), full ripe, and overripe stages, the majority of sulfur volatiles consisted of sulfur esters. Most sulfur volatiles increased dramatically between the commercial ripe, full ripe, and overripe stages, increasing as much as 100% between full ripe and overripe. Principal component analysis indicated that sulfur volatiles could be used to distinguish overripe from full ripe and commercial ripe berries.

Analysis of the headspace composition of smokeless powders using GC–MS, GC-μECD and ion mobility spectrometry

Smokeless powder additives are usually detected from an extraction of post-blast residues or unburned powder particles followed by chromatographic analyses. This work presents the first comprehensive study of the detection of volatile and semi-volatile additives of smokeless powders using solid phase microextraction (SPME) as a sampling and pre-concentration technique. The goal of this study is to generate a list of compounds that can be used as target compounds for the vapor phase detection of smokeless powders. Sixty-five smokeless powders were studied using laboratory-based gas chromatography techniques and a field deployable ion mobility spectrometer (IMS). The detection of diphenylamine, ethyl and methyl centralite, 2,4-dinitrotoluene, diethyl and dibutyl phthalate by IMS is suggested as a method to indicate the presence of smokeless powders. A previously reported SPME-IMS analytical approach facilitates rapid sub-nanogram detection of the vapor phase components of smokeless powders. The analyte mass present in the vapor phase was sufficient for a SPME fiber to extract and concentrate most analytes at amounts above the detection limits of both the GC and the IMS methods. Analysis of 65 different smokeless powder samples revealed that diphenylamine was present in the headspace of 96% of the powders studied. Ethyl centralite was detected in 47% of the powders and 8% of the powders contained methyl centralite. Nitroglycerin was the dominant peak present in the headspace of the double-based powders. Another important headspace component, 2,4-dinitrotoluene, was detected in 44% of the powders comprising both double and single-based powders. Static headspace SPME of small amounts (∼100 mg) of smokeless powder samples for ∼5 min at room temperature resulted in the successful detection of the headspace components, demonstrating the applicability of the technique for field detection of smokeless powders using IMS as a detector.

SPME-GC/MS identification of aroma compounds in rose flowers

The content and composition of active ingredients and essential oils in medicinal and aromatic plants have been studied for several decades. The volatile compounds in essential oils have been analysed routinely using gas chromatography (GC) since 1966, and with GC coupled to mass spectrometric detection (GC/MS) since 1978.The 13 rose varieties selected for chemical analysis varied for colour, shape and fragrance. The static headspace solid phase microextraction (sHS-SPME) technique recently developed for sample preparation and sample enrichment was used to study the volatile aromatic components.The main volatile compound of a sweet-smelling purple rose was found to be phenyl ethyl alcohol (33–52%). The phenyl ethyl alcohol content of fragrant rose flowers with blackish-purple petals increased continuously from early summer to late autumn (from 17 to 70 %). The dominant aromatic components of the yellow, orange and pink rose flowers were hexanol, hexenyl acetate and benzyl alcohol. Phenyl ethyl alcohol and orcinol dimethyl ether were the main constituents of the fragrant pink and white rose varieties. Methyl vinyl anisol and orcinol dimethyl ether were dominant in rose flowers with beige petals. In summary, it can be concluded that the SPME-GC/MS method is suitable for the characterization of rose varieties and for the chemical analysis of aromatic volatile compounds.

A comparison of citrus blossom volatiles

The objective of this study was to identify the major volatiles and their relative concentrations in intact grapefruit, sweet orange, sour orange, mandarin, lemon, lime and pummelo blossoms. Volatiles from freshly picked blossoms were collected and concentrated using static headspace solid-phase microextraction and then separated and identified using GC–MS. Seventy volatiles were detected, 66 identified, of which 29 were identified for the first time in citrus blossoms. Major volatiles consisted of linalool, β-myrcene, α-myrcene, limonene, ( E)-ocimene, methyl anthranilate and indole. In terms of total volatiles: pummelo ≫ grapefruit ≈ sweet orange > sour orange ≈ mandarin ≈ lemon–lime > Volkamer lemon > Kaffir lime. Principal component analysis of blossom volatiles demonstrated that there were three widely separated, tightly clustered groups which consisted of mandarin, lemon–lime and pummelo. Other cultivars of possible mixed parentage produced non-overlapping values within the boundaries of these three clustered groups. The first two Eigenvectors explained 83% of the total variance. Linalool, limonene and myrcene had the highest loading values. Those cultivars requiring insect pollination such as pummelo produced highest levels of total volatiles as well as highest levels of known honeybee stimulants such as 1-hexanol and linalool.