Α-terpineol Research Articles

In-situ formation of a hydrophobic deep eutectic solvent based on alpha terpineol and its application in liquid-liquid microextraction of three β-blockers from plasma samples

A new microextraction procedure based on liquid-liquid microextraction using a deep eutectic solvent has been used for the extraction of three β-blockers (atenolol, propranolol, and metoprolol) from plasma samples. The enriched analytes were analyzed by gas chromatography-mass spectrometry. In this study, both of the microextraction and synthesis processes were accelerated by using microwave radiations. In this procedure, 5 mL diluted plasma sample was transferred into a glass test tube and it was mixed with 0.20 g tetramethylammonium chloride. Then 0.5 mL of dimethylformamide (as a co-disperser) was mixed with 610 µL alpha terpineol and the mixture was dispersed into the solution to form a homogenous solution. The tube was placed under microwave radiations for 1 min. By doing so, tetramethylammonium chloride-alpha terpineol deep eutectic solvent was formed in sample solution as tiny droplets and the analytes were extracted into them. Then the tube was cooled with tap water and centrifuged for 5 min at 5000 rpm. Finally 1 µL of the deep eutectic solvent was injected into the determination system. Low limits of detection (0.130–0.205 ng mL−1) and quantification (0.435–0.692 ng mL−1), high extraction recovery (72–86%), and good precision (relative standard deviation ≤ 5.3%) were obtained. The introduced method was effectively applied for determination of the β-blockers’ concentrations in plasma samples.

Essence aromatique du Géranium Odorant (Pelargonium graveolens L’Hérit.) d’Algérie : exploration des propriétés antioxydante, anti-inflammatoire et anticancéreuse (anti-angiogénique et cytotoxique), in vitro et in ovo, vis-à-vis de différentes lignées cellulaires cancéreuses métastasiques

The study of natural products is one of the strategies implemented for the discovery of new compounds that can be used in cancer therapy. Aromatic herbs and medicinal plants found in Algeria and their anti-angiogenesis and cytotoxic potentials against cancer have not been much explored. Our work aimed to evaluate the antioxidant, anti-inflammatory and anticancer properties of the essential oil (EO) extracted from rose-scented geranium (Pelargonium graveolens) and its major (citronellol) and characteristic (linalool) constituents. The chemical composition of EO was determined with chromatographic analysis and revealed the presence of citronellol as the major compound (25.84%). A strong chelating power of terpene alcohols (IC50=1.58±0.23mg/mL for citronellol) was found, with a significant difference (P<0.05) compared with the standard antioxidants used (L-ascorbic acid and butylated hydroxyanisole). The EO is distinguished by an interesting anti-inflammatory effect with the lowest IC50 (4.63±0.3mg/mL), and it constitutes a good stabilizer of the erythrocyte membrane. Citronellol also exhibited the best anti-inflammatory effect (IC50=0.74±0.09mg/mL). We also assessed the anticancer effect of EO on two main pathways involved in cancer development, angiogenesis and cell proliferation, using in ovo bioassays with a chorio-allantoic membrane (CAM) of chicken eggs and in vitro assays of its cytotoxicity on different metastatic breast cancer (MDA-MB-231), gastric (AGS) and melanoma (MV3) cell lines. In the CAM model, the density of micro-vessels is 75±10in the group supplemented with EO compared to 140±9for the control group (b-FGF). In addition, the EO significantly reduced the number of newly formed vessels. The cytotoxicity was evaluated using the cell proliferation inhibition method and cell viability was measured using the MTT test. Results revealed that the treatment of cancer lines with different concentrations of EO reduces the rate of cell viability in a dose-dependent manner. EO showed the greatest cytotoxicity on the AGS line with an inhibition rate of 92.87±0.13% at the highest dose (4μL/mL), followed by the MV3line (88.76±0.96%). Data demonstrated that rose-scented geranium EO has an antitumor potential on metastatic cancer cell lines. It is distinguished by its antiproliferative, anti-angiogenic, and anti-inflammatory activities. Medicinal plants might contain new molecules, with new structures, which could become lead candidate among future anticancer drugs.

Theoritical evaluation of Citrus Aurantium leaf extract as green inhibitor for chemical and biological corrosion of mild steel in acidic solution: Statistical, molecular dynamics, docking, and quantum mechanics study

Citrus Aurantium extract consists of many compounds such as Alpha terpineol (AT), Linalool (LI), Linalyl acetate (LA), and Monoterpene hydrocarbons (MH) that suggested as corrosion inhibitors in the ground and protonated states. The current study included treatment of the corrosion process caused by the aggressive ions and/or Acidithiobacillus ferrooxidans bacteria (A. ferrooxidans) through Density Function Theory (DFT). The autodock process was carried out by the Molecular Graphic Laboratory (MGL) and Discovery Studio Visualizer (DSV) software. The bond length, angles, and dihedral were measured to present the adsorption sites of molecules. Also, the HOMO, LUMO, dipole moment, energy gap, and more parameters were used to compare the efficiency of the inhibitors. Total Electron Density (TED) and Electrostatic Surface Potential (ESP) were used to show the sites of adsorption according to electron density. Fukui function used to present the ability of atoms to donate and receipt electrons. Binding energy (Eb) was used to test the inhibition ability of A. ferrooxidans by docking calculations. DFT showed that the order of corrosion inhibition was MH > LI > LA > AT, while bio-corrosion inhibition of A. ferrooxidans was AT > MH > LA > LI. Statistical analysis was used to correlate quantum chemical parameters with inhibition efficiency. A significant model was obtained with a 0.98 correlation coefficient. The calculated inhibition efficiency was compared with the experimental one.

Exploring the multisensory perception of terpene alcohol and sesquiterpene rich hop extracts in lager style beer

Understanding the contribution of hop essential oil to the multisensory profile of beer is known to be challenging because of its chemical and sensory complexity. Limited research has been conducted investigating hop-derived volatiles' role in the modulation of taste and mouthfeel sensations. Supercritical CO₂ can be used to extract specific fractions from hop oil, thereby enabling the localisation of compounds responsible for different sensory impressions. Terpene alcohol and sesquiterpene fractions were extracted from a Magnum hop oil and further fractionated into seven sub-fractions and individual compounds. All extracts were evaluated in lager (4.5% v/v) by a trained panel (n = 10) using a newly developed attribute lexicon and following a sensory descriptive analysis approach. The sensory data was analysed using ANOVA, followed by Tukey’s test (HSD) and correlated with chemical profile data obtained by gas chromatography-mass spectrometry (GC–MS) by Principal Component Analysis. The study revealed evidence for hop extracts to impart multisensory characteristics to beer due to sensory interactions within and across modalities. The monoterpene alcohols-rich fractions and particularly geraniol, added fruity- and floral aromas and flavours, modified the sweetness and induced a smooth bitterness in the beer matrix. Flavouring the beer with sesquiterpene fractions resulted in a harsh bitterness sensation. Contrary to previous findings, the humulene epoxides fraction appeared to have limited effects on lingering bitterness and astringency, illustrating the need for temporal sensory assessments in future studies. This research shows that splitting hop oil into fractions and sub-fractions provides a source of natural, sustainable flavouring preparations with distinct sensory characteristics.

Functional characterization and substrate promiscuity of sesquiterpene synthases from Tripterygium wilfordii

Acyclic terpenes, commonly found in plants, are of high physiological importance and commercial value, and their diversity was controlled by different terpene synthases. During the screen of sesquiterpene synthases from Tripterygium wilfordii, we observed that Ses-TwTPS1-1 and Ses-TwTPS2 promiscuously accepted GPP, FPP, and GGPP to produce corresponding terpene alcohols (linalool/nerolidol/geranyllinalool). The Ses-TwTPS1-2, Ses-TwTPS3, and Ses-TwTPS4 also showed unusual substrate promiscuity by catalyzing GGPP or GPP in addition to FPP as substrate. Furthermore, key residues for the generation of diterpene product, (E, E)-geranyllinalool, were screened depending on mutagenesis studies. The functional analysis of Ses-TwTPS1-1:V199I and Ses-TwTPS1-2:I199V showed that Val in 199 site assisted the produce of diterpene product geranyllinalool by enzyme mutation studies, which indicated that subtle differences away from the active site could alter the product outcome. Moreover, an engineered sesquiterpene high-yielding yeast that produced 162 mg/L nerolidol in shake flask conditions was constructed to quickly identify the function of sesquiterpene synthases in vivo and develop potential applications in microbial fermentation. Our functional characterization of acyclic sesquiterpene synthases will give some insights into the substrate promiscuity of diverse acyclic terpene synthases and provide key residues for expanding the product portfolio.

Effects of terpene alcohol dopant on the morphology and electro‐optical properties of polymer‐dispersed liquid‐crystal composite films

AbstractTerpenes are a large class of hydrocarbon compounds derived from isoprene, which can be produced by plants or emitted by insects. Terpene alcohols contain double bonds that may affect the addition polymerization, and hydroxyl groups that can promote the network crosslinking density during the formation of polymer‐dispersed liquid‐crystal (PDLC) composite films. In this work, effects of different terpene alcohol dopant on the morphology and electro‐optical properties of PDLC films are systematically investigated. It is found that the appropriate dopant amount of geraniol (GOL) has the superior effect to improve the electro‐optical performance. The optimum addition amount is at 3 wt%, where the transmittance vs. voltage curve gets steeper, the driving voltage of PDLC film reduces from 74 to 32 V and meanwhile the contrast ratio maintains at a relatively high level (123). Thus, this work not only broadens the application scope of the natural spices but also provides a new strategy to reduce the driving voltage of PDLC films for practical applications.

Перспективные расы дрожжей для молодых игристых вин с мускатным ароматом

Introduction. In order to solve the growing demand for Muscat sparkling wines, some of the Muscat grapes used for the production of liqueur wines should be used as a raw material for sparkling wines. The technology of preparing young sparkling wines has a shorter production cycle. Science-based selection of the yeast race makes it possible to obtain young sparkling wines with a clear and bright Muscat aroma.&#x0D; Study objects and method. The research featured young sparkling wines from White Muscat grapes, produced using different yeasts races. The research involved both standard and modified methods of enochemical analysis.&#x0D; Results and discussion. The LALVIN QA-23 and Odesskiy Cherniy-SD-13 yeast races demonstrated a more active fermentation of Muscat white wort. The Sevastopolskaya 23 sample had in a slower fermentation, which promoted a greater accumulation of bound forms of carbon dioxide (16%). It contained the smallest amount of residual sugars (2 g/dm3) and thriable acids (6 g/dm3) and the largest amount of polyphenols (103 mg/dm3) and amine nitrogen (91 mg/dm3). Two samples accumulated a sufficient amount of free terpenes: 1.16 mg/dm3 for LALVIN QA-23 and 1.13 mg/dm3 for Sevastopolskaya 23. The degustation scores were quite high: LALVIN QA-23 received 9.03 points and Odesskiy Cherniy-SD-13 – 9.02 points, while Sevastopolskaya 23 scored 9.00 points. The LALVIN QA-23 sample proved to have the most pronounced varietal aroma, whereas the Odesskiy Cherniy-SD-13 sample possessed a more complex aromatic complex.&#x0D; Conclusion. The LALVIN QA-23 and Sevastopolskaya 23 yeast races were found suitable for bottle champagnization of young Muscat sparkling wines. They accumulated a sufficient amount of terpene alcohols. The samples had a clear Muscat aroma, harmonious taste, and good typical properties. The new method makes it possible to produce high quality sparkling wines in the harvest year.

Combining Metabolic and Monoterpene Synthase Engineering for de Novo Production of Monoterpene Alcohols in Escherichia coli

The monoterpene alcohols acyclic nerol and bicyclic borneol are widely applied in the food, cosmetic, and pharmaceutical industries. The emerging synthetic biology enables microbial production to be a promising alternative for supplying monoterpene alcohols in an efficient and sustainable approach. In this study, we combined metabolic and plant monoterpene synthase engineering to improve the de novo production of nerol and borneol in prene-overproducing Escherichia coli. We engineered the growth-orthogonal neryl diphosphate (NPP) as the universal precursor of monoterpene alcohol biosynthesis and coexpressed nerol synthase (GmNES) from Glycine max to generate nerol or coexpressed the truncated bornyl diphosphate synthase (LdtBPPS) from Lippia dulcis for borneol production. Further, through site-directed mutation of LdtBPPS based on the structural simulation, we screened multiple variants that markedly elevated the production of acyclic nerol or bicyclic borneol, of which the LdtBPPSS488T mutant outperformed the wild-type LdtBPPS on borneol synthesis and the LdtBPPSF612A variant was superior to GmNES on nerol production. Subsequently, we overexpressed the endogenous Nudix hydrolase NudJ to facilitate the dephosphorylation of precursors and boosted the production of nerol and borneol from glucose. Finally, after the optimization of the fermentation process, the engineered strain ENO2 produced 966.55 mg/L nerol, and strain ENB57 generated 87.20 mg/L borneol in a shake flask, achieving the highest reported titers of nerol and borneol in microbes to date. This work shows a combinatorial engineering strategy for microbial production of natural terpene alcohols.

Matteson Reaction under Flow Conditions: Iterative Homologations of Terpenes.

The Matteson reaction is ideally suited for flow chemistry since it allows iterative homologation of boronate esters. The present study provides accurate data on reaction times of the individual steps of the Matteson reaction, which occurs in less than 10 s in total. The protocol allows terpenes to be (per-)homologated in a controlled manner to yield homo-, bishomo-, and trishomo-terpenols after oxidative workup. The new terpene alcohols are validated with respect to their olfactoric properties.

The effect of Eurotium cristatum (MF800948) fermentation on the quality of autumn green tea

Autumn green tea (AT) has poor taste quality for its strong astringency. This study aims to improve the taste quality as well as the aroma of AT by Eurotium cristatum (MF800948) fermentation and to produce a fermented autumn green tea (FT). Results showed that the aroma quality of AT was improved, and the content of terpene alcohols that impart characteristic flowery aroma to FT significantly increased. The umami intensity of FT was comparable to that of AT while the astringency tasted much weaker mainly due to the oxidation of the catechins. The results also confirmed that theabrownins exhibited strong umami taste, not astringent taste. Finally, a metabolic map was analyzed to show the effect of E. cristatum (MF800948) on the quality of AT, and to visualize the changes of differential compounds in AT and FT. The work provides insights into the quality improvement of autumn green tea.

Emissions from Heated Terpenoids Present in Vaporizable Cannabis Concentrates.

Vaporizable cannabis concentrates (VCCs) consumed as a liquid (vaping) or a waxy solid (dabbing) are becoming increasingly popular. However, their associated emissions and impacts have not been fully described. Mixtures containing different proportions of 12 VCC terpenoids and high MW compounds were heated at 100-500 °C inside a room-sized chamber to simulate emissions. Terpenoids, thermal degradation byproducts, and ultrafine particles (UFPs) were quantified in the chamber air. Air samples contained over 50% of emitted monoterpenes and less than 40% of released sesquiterpenes and terpene alcohols. Eleven degradation byproducts were quantified, including acrolein (1.3-3.9 μg m-3) and methacrolein (2.0 μg m-3). A large amount of UFPs were released upon heating and remained airborne for at least 3 h. The mode diameter increased from 80 nm at 100 °C to 140 nm at 500 °C, and particles smaller than 250 nm contributed to 90% of PM1.0. The presence of 0.5% of lignin, flavonoid, and triterpene additives in the heated mixtures resulted in a threefold increase in the particle formation rate and PM1.0 concentration, suggesting that these high-molecular-weight compounds enhanced aerosol inception and growth. Predicted UFP emission rates in typical consumption scenarios (6 × 1011-2 × 1013 # min-1) were higher than, or comparable with, other common indoor sources such as smoking and cooking.

Neuroprotection by solanesol against ethidium bromide-induced multiple sclerosis-like neurobehavioral, molecular, and neurochemical alterations in experimental rats

Background: Multiple Sclerosis (MS) is an idiopathic chronic neuroinflammatory disease characterized by neurodegeneration that clinically presents motor neuron disabilities, memory, and cognitive dysfunction. Recent findings suggest that the down-regulation of SIRT-1 associated with the progression of MS. Solanesol (SNL) is an active phytoconstituent isolated from the plant Nicotiana tobacum, belonging to the Solanaceae family and a significant biosynthetic precursor to CoQ10 with potent antioxidant and neuroprotective properties. Chemically, it is a long-chain non-cyclic terpene alcohol that consists of nine isoprene units. Purpose: In the current study, we investigated the neuroprotective potential of SNL (40–80 mg/kg) in intracerebropeduncle (ICP) ethidium bromide (EB) induced MS-like neurobehavioral alterations in Wistar rats. Methods: Wistar rats were equally divided into six groups (n = 6) and treated with 0.1%/10μl of ethidium bromide injection for seven days. Long-term treatment with SNL shows neuroprotective potential by improving motor function, grip strength, memory and cognition. Results: Our findings are primarily related to the upregulation of SIRT-1 level and the myelin basic protein in the brain. In addition, SNL also modulates the level of apoptotic markers (caspase-3, Bax, Bcl-2) with mitochondrial-ETC complex dysfunction in the rat brain. Further, SNL decreased inflammatory cytokines (TNF-α, IL-1β), oxidative stress markers, and restored neurotransmitter levels. Our findings also reveal the neuroprotective effect of SNL by restoring gross pathological alterations and reducing the volume of demyelination in rats. Thus, the present study concludes that SNL as a SIRT-1 signaling activator has neuroprotective potential against EB-induced MS rats. Hence, SIRT-1 signaling may be an effective therapeutic target strategy for the treatment of MS. However, more investigations are needed to be carried out to prove these beneficial effects.

Chemometrics-based aroma profiling for revealing origin, roasting indices, and brewing method in coffee seeds and its commercial blends in the Middle East

Coffee is among the most consumed beverages worldwide. The present study reports on the aroma composition associated with coffee seeds brewing. Aroma of authentic coffee specimens of Coffea arabica and C. robusta alongside with typical products consumed in the Middle East were analyzed using HS-SPME coupled with GC–MS. In addition, multivariate data analysis (MVA) was employed. Results revealed for 102 volatiles with a distinct aroma profile between the different brewing methods. Infusion demonstrated higher esters level, while decoction and maceration were more abundant in sesquiterpenes and terpene alcohols, respectively. Besides, heat-induced products, i.e., 4-vinyl guaiacol was identified as potential roasting index in instant coffee and roasted C. robusta brews. Blending with cardamom further masked the smoky odor of such compounds by its fragrant terpinyl acetate. This study provides the first report on the chemical sensory attributes of Middle Eastern coffee blends and further reveal for the impact of brewing, roasting on its aroma composition.

Vanadium-doped sodium phosphomolybdate salts as catalysts in the terpene alcohols oxidation with hydrogen peroxide.

In this work, we have explored the catalytic activity of Keggin-type heteropolyanions PMo12−nVnO40(3+n)− (n = 0, 1, 2, or 3) in the form of sodium salts in green oxidation routes of terpene alcohols with hydrogen peroxide. Nerol was the model molecule selected to assess the impacts of the main reaction parameters, such as temperature, catalyst load, and stoichiometry of reactants. The impacts of the presence of vanadium at different proportions (i.e., V1, V2, and V3 loads/per anion) in the structure of phosphomolybdate catalysts were assessed. All the catalysts were characterized by various techniques such as powder X-ray diffraction, attenuated diffuse reflectance infrared spectroscopy, ultraviolet-visible spectroscopy, thermogravimetric analysis, isotherms of adsorption–desorption of N2 measurements of surface area, scanning electronic microscopy, energy-dispersive X-ray spectroscopy, and n-butylamine potentiometric titration. Among the catalysts assessed, Na4PMo11VO40 was the most active and selective toward epoxides. The efficiency of this catalyst in the epoxidation of different terpene alcohols was investigated. Special attention was dedicated to correlating the composition and properties of the vanadium-doped phosphomolybdic catalysts with their catalytic activity.

Terpene alcohol and phytosterol from the root of the Commelina Diffusa Burm. F

Commelina diffusa Burm. f. (C. diffusa) is the richest bio-resource of drugs of traditional systems of medicine, modern medicines, nutraceuticals, food supplements, folk medicines, pharmaceutical intermediates and chemical entities for synthetic drugs. This study aims to isolate and characterize compounds from the methanol extract of the plant. Healthy roots of the plant were collected, chopped into small pieces, air-dried under a shade, segregated, pulverized, extracted with methanol using maceration technique and concentrated to obtain the plant extract. The results from the phytochemical screening of the plant extract revealed the presence of higher amount of steroids, terpenoids, alkaloids, phenolic compounds, tannins, saponins, amino acid and phytosteroids. While column chromatography was used for the isolation and purification of the pure compound. Silica gel chromatographic separation of the CH3OH extract gave stigmasterol and 3, 7, 11, 15-Tetramethyl-2-hexadecen-1-ol. A complete characterization of the isolated compound was done with the help of (UV-Vis, IR, 1D NMR) spectroscopic techniques.

Use of Raman Spectroscopy for Analysis and Detection of Some Sudanese Edible Oils

Vegetable edible oils provide high nutritional and health value in the Sudanese diet. It is also used in the pharmaceutical industry and an essential ingredient in cosmetics. This paper reviews the use of Raman spectroscopy for the analysis, quality and characterization of edible oils, including six types of oils (corn, extra virgin olive, sunflower, factory sesame, presses sesame, and peanut) purchased from local Sudanese stores. The results showed that the spectra of edible oils are similar, but they show some differences that, despite their smallness, allow them to be distinguished from each other. Divide the spectrum into the fingerprint region. The range ranges between (600 and 1800) cm^-1 the silent region", this spectral region is (1800 to 2500) cm^-1, and range is from (2500 to 3400) cm^-1, known as the "high wave number region". Raman spectra also pliable the determination of the degree of saturation and unsaturation of oils. This characteristic is related to the value of iodine, and the degree of unsaturation can be used to classify and approve oils, which is especially useful with high-quality oils in the appearance of the vibration modes at 1155 cm^-1 and 1525 cm^-1. Adulteration of edible oils with cheaper oils is a major concern in the oil industry. The capabilities of a Raman spectrometer were checked to assess the purity of the samples (peanut spectrum and presses sesame spectrum). Raman spectroscopy allowed the examination of secondary components such as sterols, hydrocarbons, terpene alcohols and polyphenols. Raman spectroscopy is used because this innovative method provides fast, non-destructive and reagent-free measurements, samples do not need to be processed and do not require large volumes.

Dysprosium-doped zinc tungstate nanospheres as highly efficient heterogeneous catalysts in green oxidation of terpenic alcohols with hydrogen peroxide

Dysprosium-doped zinc tungstate nanospheres efficiently catalyzed the epoxidation of terpenic alcohols using hydrogen peroxide, an inexpensive and environmentally benign oxidant.

IMPROVEMENT OF THE TECHNOLOGICAL MODES OF PRODUCING DRY WHITE TABLE WINES

By using the classical technology of making dry white wines, which does not involve maceration of the pomace, we can produce standard table wines, light and delicate. This minimises such an objectionable factor as saturation of the wine with extra nitrogenous and phenolic substances and oxidative enzymes. On the other hand, this scheme gives a specific varietal aroma no chance to reveal itself more expressively. The paper overviews briefly the scientific works considering the modes of pomace maceration before fermentation and the use of enzyme preparations in the technology of white table wines. The physicochemical and sensory characteristics of wine materials from Rkatsiteli grapes grown in the south of the Mykolaiv Region have been analysed. This analysis has proved that standard white table wine materials can be obtained both by the traditional method (the so called ‘white’ method) and with the use of short-term maceration of the pomace. Macerating the pomace resulted in obtaining fuller, richer wine materials with a bright aroma and good body. It has been shown that to obtain bright and not too blunt wine materials, the most essential parameter of the maceration process is its low temperature. A pectolytic enzyme preparation used during maceration increased, to some extent, the mass concentration of phenolic substances, the reduced extract, the optical density, and the concentration of terpene alcohols. Besides, it allowed fuller revealing a wine’s aromatic profile. The research has resulted in establishing that there is regularity in how the concentration of terpene alcohols changes with different temperature conditions of steeping the pomace. It has been shown that the maximum concentration of terpenes responsible for the varietal aroma is best retained in wine materials when the maceration temperature is 5°C. A rise in the pomace maceration temperature to 20°C led to a decrease in the concentration of labile terpene alcohols, so it should be avoided in producing quality wines. Studying different maceration modes has allowed recommending a certain method to manufacture full-bodied, well-structured white table wines with a pronounced varietal aroma. This method involves adding the enzyme preparation Depectil CLARIFICATION to the pomace and macerating it for 12 hours at 5°C.

Thin layer chromatography based extraction approaches for improved analysis of volatile compounds with gas chromatography-mass spectrometry and direct analysis with gas analyzer.

In this study, thin-layer chromatography was applied for selective extraction of volatile compounds in perfume prior to analysis with solid phase microextraction and gas chromatography-mass spectrometry. The standard compounds were desorbed from the thin-layer chromatography plate and extracted at 80°C for 15min showing good linearity of the calibration curves (R2 >0.98) and acceptable recovery range (65-81%). The plate after the separation was cut into four smaller parts followed by solid phase microextraction/gas chromatography-mass spectrometry analysis, which revealed different compound profile in each part with the correlation between log P of the standard compounds and their positions along the thin-layer chromatography plate (R2 =0.65). This approach was applied to analyze perfume compounds in the sample with strong matrix interference from the synthetic agarwood. Terpene hydrocarbons (woody-based odors), ketones/esters, aldehydes, ethers, and alcohols were mostly observed at 8±1, 6±1, 5±2, 4±2, and 3±2cm, respectively, from the bottom of the thin-layer chromatography plate. While, the conventional solid phase microextraction/gas chromatography-mass spectrometry analysis of this sample solution revealed only 62 compounds (including 35 perfume compounds), the four-piece approach resulted in 109 compounds (62 perfume compounds). Furthermore, the capability of thin-layer chromatography-Gas Analyzer approach to analyze the isomers in this complex sample was demonstrated.

The study of the composition of the lipophilic hop extract for using in the composition of finished dosage forms

In the industrial production of the hop infructescence dry extract, the non-polar fraction in the form of a lipophilic extract obtained by extraction with heptane or hexane remains as a waste. The lipophilic extract obtained under such conditions is characterized by a significant content of biologically active substances from the groups of terpene alcohols, aldehydes, ketones, epoxides, acids, and esters. In this case, it is promising to use the lipophilic extract in further research on the development of new drugs, and it will also provide a comprehensive treatment of hop infructescences.Aim. To study the chemical composition of the lipophilic hop extract by gas chromatography for further standardization and use as a constituent of finished dosage forms.Materials and methods. The lipophilic hop extract was obtained at the SPC “Borshchagovsky CPP”, Kyiv. The chemical composition of the lipophilic fraction of hop infructescences was studied according to the requirements of the State Pharmacopoeia by gas chromatography with a flame ionization detector using an Agilent 7890 GC gas chromatograph with a 597 Agilent GC/MSD mass spectrometric detector.Results. According to the results of the studies conducted, using library spectra, 47 volatile compounds were identified in the lipophilic hop extract. The main components were (S)-3-ethyl-4-methylpentanol, 1,3,3-trimethyl-bicyclo [2,2,1] heptane-2-one, eicosamethyl-cyclodecasiloxane, 4-pentene-2-ol, Z-7-hexadecanoic acid, phthalic acid esters, 7-tetradecenal, CIS-11-hexadecenal, their content reached 75% of the area of all peaks of substances.Conclusions. In the lipophilic hop extract, the content of volatile substances has been identified and quantified by gas chromatography with a mass spectrometric detector. The major representatives of the substances are (S)-3-ethyl-4-methylpentanol and 1,3,3-trimethyl-bicyclo[2,2,1]heptane-2-one, their content is 49.5 % of the total amount of substances.