Search Results (30)

This study investigated the individual and synergistic impacts of arbuscular mycorrhizal fungi (AMF) inoculation and foliar-applied silicon nanoparticles (SiNPs) on the yield parameters, volatile profile, and phenolic composition of two Rosa damascena genotypes (D231 and C193). Experiments were conducted using a split–split–plot design, involving AMF inoculation (main plot), three SiNPs concentrations (subplot), and two rose genotypes (sub-subplot). The results demonstrated that AMF, SiNPs, and genotype all had significant and interactive effects on flower yield parameters. Foliar application of SiNPs, particularly when combined with AMF inoculation, consistently enhanced flowering parameters, including flower size, number, and weight across both genotypes. High-performance liquid chromatography (HPLC) further confirmed that phenolic acids (vanillic acid and rutin) increased following foliar application of SiNPs and AMF root colonization, particularly in genotype C193. SPME-Arrow analysis revealed that alcohols, ketones, and terpenes were the predominant volatile constituents. Phenethyl alcohol was the most abundant compound, accounting for approximately 84.69% of the total aroma content and contributing significantly to the ‘rose’ aroma. Other major volatiles included 2-undecanone (4.42%), benzyl alcohol (2.97%), and citronellol (1.95%); however, their levels varied depending on treatment and genotype. These findings highlight that the combined application of AMF and SiNPs offers a sustainable approach to enhancing both the quantitative yield and qualitative phytochemical composition (essential oil components and phenolic compounds) of R. damascena, providing a scientific foundation for optimizing its production in organic farming systems. Full article

Odorous emissions from hot-mix asphalt (HMA) plants are a growing environmental concern, particularly due to airborne aldehydes and ketones, which have low odor thresholds and a strong sensory impact. This study presents a field-ready analytical method for monitoring odor-active volatile compounds. The system uses dynamic solid-phase microextraction (SPME and SPME Arrow) with on-fiber derivatization via O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine (PFBHA) and is coupled to gas chromatography–mass spectrometry (GC–MS) for direct detection. A flow-cell sampling unit enables the real-time capture of aliphatic aldehydes and ketones under transient emission conditions. Calibration using permeation tubes demonstrated sensitivity (limits of detection (LODs) below 0.13 μg/m³), recovery above 85% and consistent reproducibility. Compound identity was confirmed using retention indices and fragmentation patterns. Uncertainty assessment followed ISO GUM (Guide to the Expression of Uncertainty in Measurement) standards, thereby validating the method’s environmental applicability. Field deployment 200 m from an HMA facility identified measurable concentrations that aligned with CALPUFF model predictions. The method’s dual-isomer resolution and 10 min runtime make it ideal for responding to time-sensitive odor complaints. Overall, this approach supports regulatory efforts by enabling high-throughput on-site chemical monitoring and improving source attribution in cases of odor nuisance. Full article

Volatile compounds greatly affect tomato aroma, but systematic analysis of volatiles in tomatoes is limited by detection techniques. Here, HS-SPME Arrow-GC × GC-Q/TOFMS was employed to analyze tomato flavor profiles across different cultivation times. To investigate the effects of light and temperature on aroma profiles, three tomato samples across different cultivation periods, including S1 (harvested on May 30th, with lowest temperature and light conditions), S2 (harvested on August 10th, with the highest temperature and light), and S3 (harvested on June 27th, with moderate temperature and light), were analyzed. Overall, 227 volatiles were identified, belonging to 9 aroma categories. Hexanal, (E)-2-hexenal, nonanal, (E)-2-Octenal, trans-geranylacetone, 6-methyl-5-hepten-2-one, 3,4-Octadiene, 7-methyl-, and citral were found to be the key volatiles contributing most significantly to differentiating the samples across cultivation periods, imparting grassy and floral–fruity notes, respectively. The S1 tomatoes had a distinct grassy aroma, whereas the S3 tomatoes had a floral/fruity fragrance. Most differential metabolites were correlated with fatty acid, amino acid, and isoprenoid pathways. S1 tomatoes were characterized by fatty aldehydes (mainly C6/C9), and S2 tomatoes contained high concentrations of fatty alcohols. S3 tomatoes were positively correlated with isoprenoid-derived volatiles. These variations might be caused by the fluctuations in daily temperature and light intensity. This work establishes a foundational reference for assessing environmental effects on tomato flavor profiles. Full article

Indigenous grape varieties from the Hrvatska Istra subregion (Croatia) represent a significant proportion of regional wine production. In this study, the potential of six indigenous varieties—Malvazija istarska, Garganja, Duranija, Surina, Hrvatica, and Teran—for the traditional method for the production of sparkling wines was evaluated. Several of these varieties are currently underutilized or neglected in contemporary viticulture. A total of 85 volatile aroma compounds, including acids, alcohols, esters, C13-norisoprenoids, and terpenes, were identified and quantified using SPME-Arrow-GC/MS. Sensory evaluation was conducted using a structured nine-point hedonic scale. Among the compounds identified, C13-norisoprenoids (notably β-damascenone, TPB, and TDN) and esters (including ethyl 3-methylbutanoate, ethyl butanoate, and ethyl hexanoate) were found to contribute most significantly to the overall aromatic profile of the sparkling wines. Sensory profiles varied distinctly among the varieties. Some varieties demonstrated pronounced aromatic and structural characteristics, making them suitable for monovarietal sparkling wine production, while others exhibited complementary sensory properties more appropriate for cuvées. This study represents the first comprehensive chemical and descriptive sensory profiling of sparkling wines produced from these Istrian indigenous grape varieties. These findings aim to support their valorization and integration into the broader spectrum of sparkling wine production, thereby enhancing their recognition and market potential. Full article

Background and Objective: The global population is struggling with significant health challenges, among which overweight and obesity stand out. Currently, 61% of adults and 7.5% of children and adolescents are affected, underscoring the urgent need for effective solutions. This study evaluated appetite-reducing prototypes related with food products, focusing on their ability to influence appetite through the sense of smell. The objective was to determine the effectiveness of these prototypes and identify the most promising candidates for further research. Methods: A questionnaire-based consumer survey was performed for six appetite-reducing agents. Forty-five participants with elevated body mass index values (BMI ≥ 25) were asked to verify the samples in terms of aroma intensity, pleasure, and potential for appetite reduction. Also, qualitative parameters such as the identification of the samples’ food associations was performed within the questionnaire. The questionnaire results were further compared with headspace solid-phase microextraction (HS-SPME Arrow) analysis results to identify volatile organic compounds associated with appetite-reducing properties. Results: The proof-of-concept study revealed that prototypes with unpleasant and irritating aromas demonstrated the highest appetite-reducing potential, scoring approximately 24 out of 35 points. Conversely, prototypes with pleasant, dessert-like aromas showed lower effectiveness, scoring between 14 and 18 points. Conclusions: By linking consumer perceptions to chemical analyses, we identified effective prototypes for further investigation, including studies measuring actual food intake. These findings contribute to developing innovative, non-invasive strategies to address overweight and obesity, offering a new dimension to appetite control through sensory modulation. Full article

A portable mass spectrometer (PMS) was combined with a mesoporous silica material (SBA-15) coated solid-phase microextraction (SPME) Arrow to develop a rapid, easy-to-operate and sensitive method for detecting five veterinary drugs—amantadine, thiabendazole, sulfamethazine, clenbuterol, and ractopamine—in milk and chicken samples. Equipped with a pulsed direct current electrospray ionization source and a hyperboloid linear ion trap, the PMS can simultaneously detect all five analytes in approximately 30 s using a one-microliter sample. Unlike traditional large-scale instruments, this method shows great potential for on-site detection with no need for chromatographic pre-separation and minimal sample preparation. The SBA-15-SPME Arrow, fabricated via electrospinning, demonstrated superior extraction efficiency compared to commercially available SPME Arrows. Optimization of the coating preparation conditions and SPME procedures was conducted to enhance the extraction efficiency of the SBA-15-SPME Arrow. The extraction and desorption processes were optimized to require only 15 and 30 min, respectively. The SBA-15-SPME Arrow–PMS method showed high precision and sensitivity, with detection limits and quantitation limits of 2.8–9.3 µg kg⁻¹ and 10–28 µg kg⁻¹, respectively, in milk. The LOD and LOQ ranged from 3.5 to 11.7 µg kg⁻¹ and 12 to 35 µg kg⁻¹, respectively, in chicken. The method sensitivity meets the requirements of domestic and international regulations. This method was successfully applied to detect the five analytes in milk and chicken samples, with recoveries ranging from 85% to 116%. This approach represents a significant advancement in food safety by facilitating rapid, in-field monitoring of veterinary drug residues. Full article

The leaves of Ilex paraguariensis (known as Yerba mate), used as a popular beverage, are a very well-recognized plant material with various biological activities, including analeptic (because of caffeine), anti-obesity (phenolics, saponins), antimicrobial, and antiviral (phenolics, saponins). Here, the chemical compositions of the leaves of two European Ilex species (× meserveae and aquifolium) with three varieties each were investigated. The terpenoid, saponin, and polyphenolic fractions were submitted for LC-MS or GC-MS analysis against a standard Mate leaf. In addition, the aroma profiles of all the species were analysed using HS-SPME-Arrow prior to GC-MS analysis. All fractions were subjected to antiviral and cytotoxic assays. We found 86 compounds in all accessions, with limonene, linalool, and p-cymene being predominant. There were minor similarities between the volatile compositions of the European and South American species. We found ursolic and oleanolic acid to be the main compounds in the terpenoid fraction. Mono-caffeoylquinic acids and di-caffeoylquinic acids were the main constituents of the polar fractions. About 180 compounds from the saponin group were tentatively identified, of which 9 and 3 were selected as distinctive markers for I. meserveae and I. aquifolium, respectively. Based on chemical screening, I. aquifolium Silver Queen was chosen as the source of terpenoid and saponin fractions and polyphenol extracts. The most substantial inhibition of cancer cell growth was observed with saponin in the case of the MCF7 (human breast cancer) cell line, while for LoVo and L929 cell lines (human colorectal cancer and reference mouse fibroblasts), it was slightly weaker. These results should be analysed further as a promising chemoprevention of colorectal and gastrointestinal cancers. Saponin and polyphenolic extracts exhibited similar activities against HSV-1 and HAdV-5, with 4-log reduction in virus titres. This study focuses our attention on a field of potential antiviral formulations derived from European holly. Full article

This research aimed to analyze the impact of two different non-Saccharomyces yeast species on the aromatic profile of red wines made from the cv. Babić (Vitis vinifera L.) red grape variety. The grapes were obtained from two positions in the Middle and South of Dalmatia. This study compared a control treatment with the Saccharomyces cerevisiae (Sc) strain as a type of sequential inoculation treatment with Lachancea thermotolerans (Lt x Sc) and Torulaspora delbrueckii (Td x Sc). The focus was on the basic wine parameters and volatile aromatic compound concentrations determined using the SPME-Arrow-GC/MS method. The results revealed significant differences in cis-linalool oxide, geraniol, neric acid, and nerol, which contribute to the sensory profile with floral and rose-like aromas; some ethyl esters, such as ethyl furoate, ethyl hexanoate, ethyl lactate, ethyl 2-hydroxy-3-methylbutanoate, ethyl 3-hydroxy butanoate, diethyl glutarate, and diethyl succinate, contribute to the aromatic profile with fruity, buttery, overripe, or aging aromas. A sensory evaluation of wines confirmed that Td x Sc treatments exhibited particularly positive aromatic properties together with a more intense fullness, harmony, aftertaste, and overall impression. Full article

Damask rose (Rosa damascena Mill.) is an aromatic industrial plant with different applications. Selection of cultivars with high-value metabolites such as flavonoids—with acceptable yields—can lead to elite cultivars for mass propagation in various industries. A field experiment was carried out in a randomized complete block design (RCBD) to evaluate metabolites and some yield-related morphological data. In the present investigation, for the first time 13 flavonoid components of nine Iranian damask rose cultivars were compared using LC-MS/MS. As a result, 13 flavonoids were identified, most of which were reported for the first time in rose petals. Phloridzin (72.59–375.92 mg/100 g dw), diosmetin (82.48–153.16 mg/100 g dw) and biochanin A (0–1066.89 mg/100 g dw) were the most abundant, followed by trans-chalcone (0–106.29 mg/100 g dw) and diosmin (41.55–84.57 mg/100 g dw). Levels of naringenin also ranged from 3.77 in B111 to 54.70 mg/100 g dw in C294, while luteolin varied from 4.37 in B111 to 28.87 mg/100 g dw in C294. The SPME Arrow technique also was applied to determine the real aroma of the studied cultivars. Phenethyl alcohol was the most abundant compound, in the range of 69.28 to 77.58%. The highest citronellol/geraniol (C/G) was observed in D234 (4.52%) and D237 (4.30%), while the lowest amount belonged to A104 (1.28%). Rose oxide, as the most crucial factor for odor, ranged from 0.06% in D237 to 0.15% in D211. Based on cluster and principal component analysis (PCA), D234 cultivar can be suggested as a promising cultivar with high yield, high C/G content and high rose oxide, while D234 and C294 were the most valuable cultivars in terms of flavonoids with high yield. Finally, these cultivars can be introduced for further breeding programs and industrial cultivation. Full article

Hemp is used as a source of fiber, oil and bioactive substances including volatile and cannabinoid-containing substances. This paper presents, for the first time, results on the evaluation of drying methods (convective, vacuum–microwave and combined convective pre-drying and vacuum–microwave finishing drying) of hemp leaves on the qualitative and quantitative changes in secondary metabolites, including essential oils, cannabinoids and sterols. A ranking and descriptive test of hemp leaves was also performed. Drying kinetics was presented using three models, including logarithmic, Midilli and modified Page. The SPME-Arrow technique was used to determine 41 volatile compounds, of which caryophyllene, β-myrcene and α-humulene were dominant in dried and fresh leaves. Regarding the essential oils obtained, 64 were identified, with caryophyllene, humulene epoxide II and limonene being the dominant ones. For preserving the highest amount of oils, the best method was the convective pre-drying followed by vacuum–microwave finishing drying (CD60-VMD) combined method, where the retention of volatile compounds was 36.08%, whereas the CD70 and 240-VMD methods resulted in the highest loss of 83%. The predominant cannabinoids in fresh hemp leaves were CBDA 6.05 and CBD 2.19 mg g⁻¹. Drying caused no change in the cannabinoid profile of the plant material. β-Sitosterol, campesterol and lupeol were dominant in the phytosterol and triterpene fractions. No changes in either quality or quantity were observed in any of the variants found. Full article

Volatile organic compounds (VOCs) from wood and wood composites are important contributors to odor profiles of indoor environments and can significantly influence human health and well-being. GC-MS/FID and gas chromatography (GC) with olfactometric detection (GC-O) are employed for the identification and characterization of odorants. Four different sample preparation methods are evaluated on wood strands and isocyanate adhesive–based oriented strand boards (OSBs) made from Pinus sylvestris L.: among these, dynamic headspace extraction thermal desorption ((dynamic) HS-TD), head space solid phase microextraction (HS-SPME), head space solid phase microextraction Arrow (HS-SPME Arrow), and liquid injection of a CH₂Cl₂ solvent extract. The olfactometric investigation revealed over 30 odor-active substances of cyclic and acyclic monoterpene, monoterpenoid ketone, monoterpenoid aldehyde, monoterpenoid alcohol, monoterpenoid ester, aliphatic aldehyde, alcohol, and acid and phenolic chemistry. Compared to liquid injection, (dynamic) HS-TD was found to result in a similar number of odorants (20 vs. 24), whereas HS SPME Arrow shows good performance with minimal instrumental effort, notably for monoterpene and aldehyde compounds. Native wood vs. OSB showed high concentrations of saturated and unsaturated aldehydes for the wood board sample. These findings demonstrate the capability of headspace methods for odorant detection and their suitability for standardization towards a database for wood and wood composites. Full article

Formaldehyde (FA) is a toxic compound and a human carcinogen. Regulating FA-releasing substances in commercial goods is a growing and interesting topic: worldwide production sectors, like food industries, textiles, wood manufacture, and cosmetics, are involved. Thus, there is a need for sensitive, economical, and specific FA monitoring tools. Solid-phase microextraction (SPME), with O-(2,3,4,5,6-pentafluorobenzyl)-hydroxylamine (PFBHA) on-sample derivatization and gas chromatography, is proposed for FA monitoring of real-life samples. This study reports the use of polydimethylsiloxane (PDMS) as a sorbent phase combined with innovative commercial methods, such as multiple SPME (MSPME) and cooling-assisted SPME, for FA determination. Critical steps, such as extraction and sampling, were evaluated in method development. The derivatization was performed at 60 °C for 30 min, followed by 15 min sampling at 10 °C, in three cycles (SPME Arrow) or six cycles (SPME). The sensitivity was satisfactory for the method’s purposes (LOD-LOQ at 11-36 ng L⁻¹, and 8-26 ng L⁻¹, for SPME and SPME Arrow, respectively). The method’s linearity ranges from the lower LOQ at trace level (ng L⁻¹) to the upper LOQ at 40 mg L⁻¹. The precision range was 5.7–10.2% and 4.8–9.6% and the accuracy was 97.4% and 96.3% for SPME and SPME Arrow, respectively. The cooling MSPME set-up applied to real commercial goods provided results of quality comparable to previously published data. Full article

According to the WHO, the number of overweight people (BMI ≥ 25) and obese people (BMI ≥ 30) is constantly growing. On the other hand, the number of elderly people (≥60 years old) in 2020 reached 1.4 billion worldwide. Both mentioned groups demonstrate their individual and characteristic appetite disorders. In light of the side effects of appetite stimulating drugs, which interfere with diabetics, hypertension and thrombosis medicines or diet supplements with doubtful effectiveness in reducing appetite, new and natural alternatives are highly demanded. Therefore, the present study focusses on the search for natural food aromas, which may have potential for appetite regulation. A survey was carried out among consumers with excess body weight (BMI ≥ 25) and the elderly (≥60 years old). Food products and meals pointed out by the survey participants were subjected to volatile analysis by HS-SPME Arrow followed by GC-MS. As a result, a group of volatiles and their odor characteristic were determined for appetite stimulation or reduction, which may suggest that the actual composition of food aroma is more significant than the character of the aroma. Those results may be a basis for designing appetite regulating agents, in which the mechanism of action will be based only on olfaction activity. Full article

In the present feasibility study, SPME Arrow-GC-MS method coupled with chemometric techniques, was used for investigating the impact of two different storage conditions, namely freezing and refrigeration, on volatile organic compounds (VOCs) of different commercial breads. The SPME Arrow technology was used as it is a novel extraction technique, able to address issues arising with traditional SPME fibers. Furthermore, the raw chromatographic signals were analysed by means of a PARAFAC2-based deconvolution and identification system (PARADISe approach). The use of PARADISe approach allowed for an efficient and rapid putative identification of 38 volatile organic compounds, including alcohols, esters, carboxylic acids, ketones, and aldehydes. Additionally, Principal Component Analysis, applied on the areas of the resolved compounds, was used to investigate the effects of storage conditions on the aroma profile of bread. The results revealed that the VOC profile of fresh bread is more similar to the one of bread stored in the fridge. Furthermore, there was a clear loss of aroma intensity in frozen samples, which could be explained by phenomena related to different starch retrogradation that occurs during freezing and refrigeration. However, considering the limited number of investigated samples, this study must be considered as a proof of concept; a more statistically representative sampling and further examinations of other properties, such as bread texture, need to be performed to better understand whether samples destined for eventual analysis should be frozen or refrigerated. Full article

Canines can identify prostate cancer with high accuracy by smelling volatile organic compounds (VOCs) in urine. Previous studies have identified VOC biomarkers for prostate cancer utilizing solid phase microextraction (SPME) gas chromatography–mass spectrometry (GC-MS) but have not assessed the ability of VOCs to distinguish aggressive cancers. Additionally, previous investigations have utilized murine models to identify biomarkers but have not determined if the results are translatable to humans. To address these challenges, urine was collected from mice with prostate cancer and men undergoing prostate cancer biopsy and VOCs were analyzed by SPME GC-MS. Prior to analysis, SPME fibers/arrows were compared, and the fibers had enhanced sensitivity toward VOCs with a low molecular weight. The analysis of mouse urine demonstrated that VOCs could distinguish tumor-bearing mice with 100% accuracy. Linear discriminant analysis of six VOCs in human urine distinguished prostate cancer with sensitivity = 75% and specificity = 69%. Another panel of seven VOCs could classify aggressive cancer with sensitivity = 78% and specificity = 85%. These results show that VOCs have moderate accuracy in detecting prostate cancer and a superior ability to stratify aggressive tumors. Furthermore, the overlap in the structure of VOCs identified in humans and mice shows the merit of murine models for identifying biomarker candidates. Full article