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A new method based on Ultraviolet spectrophotometry was developed and compared with that based on high‐performance liquid chromatography for the determination and quantification of anthraquinones in the extracts of Rhamnus purshiana bark. A validated quantitative analysis of cascaroside A, cascaroside B, emodin, and aloe‐emodin in these herbal products has been previously performed using high‐performance liquid chromatography coupled with a diode array detector. In the high‐performance liquid chromatography analysis, all the anthraquinones showed satisfactory regression (r2 > 0.98) within the test ranges, and the recovery was in the range of 94–117%. The limits of detection and quantification were 0.008–0.010 and 0.029–0.035 μg/mL, respectively. Hierarchical cluster analysis and principal component analysis showed differences in the anthraquinones determined from herbal samples. Subsequently, a simple and low‐cost ultraviolet spectrophotometric methodology for the quantitative analysis of the same compounds in the extracts was applied, and all the contents were determined. A paired t‐test confirmed that there were no significant differences between the two methods. Our results revealed that the developed method is simple and provides the ability to discriminate and control the quality of anthraquinones in herbal products. [ABSTRACT FROM AUTHOR]

The aim of the present study was to evaluate the sensory acceptability limit of refrigerated fish through a multivariate approach, involving classic physicochemical and bacteriological indicators and considering different consumer profiles. The results of the survival analysis demonstrated that, in general, consumers still considered the fish to be suitable for purchase (4.128 days of storage), despite being microbiologically unsuitable for consumption. However, the subsequent division of consumers into clusters indicated that women and individuals with high income and education levels tend to reject fish with few days of storage (3.650 days), mainly due to discoloration, despite still being microbiologically suitable for consumption. Thus, these segments present a safer behavior regarding the purchase of fresh fish. The influence of different frequencies of fish consumption and age of consumers on the assessment of fish freshness was not clarified. The responsibility for ensuring safe and healthy products at the point of sale must lie with the producers and distributors. However, improving consumers' ability to make good choices when buying fresh fish would bring social and economic benefits related to public health and to the seafood industry, because it would enable them to make relevant claims and demand their rights. [ABSTRACT FROM AUTHOR]

Electrocoagulation (EC) of a synthetic ternary dye mixture was investigated using sacrificial iron electrodes. Erionyl Red (ER), Isolan Bordeaux (IB), and Remazol Red (RR) textile dyes were used for preparing the ternary solution. Different operational parameters, including initial dye concentrations, salt amount, current density, EC time, and pH, were analyzed to optimize removal efficiency and energy consumption conditions. After EC treatment, the individual remaining dye concentrations were calculated by applying classical least squares (CLS). The fastest removed dye was RR and the obtained efficiency was the highest as compared to the other two dyes. The energy consumption was also investigated. [ABSTRACT FROM AUTHOR]

Grapeseed and chia oils are important for their fatty acids profile. Both oils are considered gourmet and due their high retail prices they are susceptible to adulteration. FT-MIR was used with chemometric analysis to identify and quantify the adulterants (sunflower and soybean oils) in grapeseed and chia oils. A ternary mixture system was designed for each oil using as adulterants sunflower and soybean oils (2-50%, w/w). Soft independent modelling by class analogy (SIMCA) discriminated adulterated samples and pure samples (100% of recognition and rejection). Partial least squares (PLS) showed the best calibration result (R2c: ≥ 0.95; SEC: 2.22-2.87) and validation (R2v: ≥ 0.99; SEP: 2.25-3.13). The models could be applied to identify and quantify two adulterants: sunflower and soybean oils in grapeseed and chia oils. [ABSTRACT FROM AUTHOR]

Background: Many studies have assessed the fingerprint and quantitative analysis of Ginkgo biloba preparations, but the fingerprint mainly focuses on flavonoid glycosides. However, according to our previous study, the differences among diverse manufacturers mainly involve organic acids. Methods: A novel reverse-phase liquid chromatography assay using diode array detection was developed for evaluating Ginkgo biloba preparations for quality based on a chromatographic fingerprint allowing the simultaneous assessment of eleven compounds, including four organic acids, six flavonol glycosides and one flavonoid aglycone. And the method was applied to 51 batches of Ginkgo biloba preparations from manufacturers in China. Chemometric approaches were performed for evaluating 51 batches of Ginkgo biloba preparations from various manufacturers. Results: The similarity values among the chromatograms of 51 samples ranged from 0.45 to 1.00, showing that the quality of Ginkgo biloba preparations produced by different manufacturers varied greatly. Data analysis of the 51 batches of GBP samples suggested significant variations of the total contents of all 11 targets, also demonstrating the quality difference of GBP samples. There were significant differences in organic acids in particular. Conclusion: Combining the chemical fingerprint and quantitative assessment revealed significant variations in the examined commercial products with regard to organic acids. Thus, this study provided a more comprehensive tool for monitoring the quality consistency of Ginkgo biloba preparations. [ABSTRACT FROM AUTHOR]

Fourier transform infrared spectroscopy (FTIR) in connection with chemometric analysis were used as a fast and direct approach to classify spray dried honey powder compositions in terms of honey content, the type of diluent (water or skim milk), and carrier (maltodextrin or skim milk powder) used for the preparation of feed solutions before spray drying. Eleven variants of honey powders containing different amounts of honey, the type of carrier, and the diluent were investigated and compared to pure honey and carrier materials. Chemometric discrimination of samples was achieved by principal component analysis (PCA), hierarchical clustering analysis (HCA), linear discriminant analysis (LDA), and partial least squares-discriminant analysis (PLS-DA) modelling procedures performed on the FTIR preprocessed spectral data for the fingerprint region (1800–750 cm−1) and the extended region (3600–750 cm−1). As a result, it was noticed that the type of carrier is a significant factor during the classification of different samples of powdered multifloral honey. PCA divided the samples based on the type of carrier, and additionally among maltodextrin-honey powders it was possible to distinguish the type of diluent. The result obtained by PCA-LDA and PLS-DA scores yielded a clear separation between four classes of samples and showed a very good discrimination between the different honey powder with a 100.0% correct overall classification rate of the samples. [ABSTRACT FROM AUTHOR]

Fourier transform infrared (FTIR) authentication coupled with chemometric evaluation is widely used in qualitative and quantitative analysis of food and agricultural products. This study aimed to characterize coconut testa flour (CTF) of five different Sri Lankan cultivars and to develop statistical models between FTIR data and parameters of CTF, wheat flour (WF) and their admixtures. Flour samples were subjected to FTIR analysis within the range of 4000–500 cm−1 and proximate data were recorded. Principal component analysis (PCA) was applied for FTIR data and models were developed using both univariate and partial-least-squares (PLS) regression to predict fat, protein, carbohydrates, moisture and level of admixture from FTIR spectra. Results showed that the spectral bands of both CTF and WF were indicative of organic functional groups associated with fat (~ 1745 cm−1), protein (~ 1655, ~ 1550 cm−1), carbohydrates (~ 3300, ~ 1065 cm−1) and moisture (~ 3300 cm−1). Spectral studies on the admixtures confirmed that proportional differences of the biomolecules had a direct influence on the variations occurring in the spectral bands. Application of PCA resulted in a clear discrimination among flour samples with a total variance of 97%. PLS regression showed more precise results than univariate regression. The precision of the developed PLS-regression predictive models was found to increase with the number of selected relevant spectral points and these models resulted in a good R2 value and low RMSEC and RMSEP values. The results of this study would be helpful for further chemical studies on authentication, product development and nutrition of CTF and WF. [ABSTRACT FROM AUTHOR]

We propose a rapid and simple method for determining penicillin antibiotics in medicines based on dispersive liquid–liquid microextraction of penicillin–Methylene Blue associates and measuring the colorimetric characteristics of the extracts using a smartphone and specialized software. The values of colorimetric parameters in the RGB system are used as an analytical signal (Ar). We develop procedures for determining the concentration of penicillin G, penicillin V, oxacillin, ampicillin, amoxicillin, and nafcillin in drugs. The limits of detection and determination are 0.2 and 0.6–0.8 μg/mL, respectively. Using chemometric analysis shortens the analysis time and visualizes the data. The data array is processed by the principal component analysis (PCA), hierarchical cluster analysis (HCA), and the k-means method using the XLSTAT software. Antibiotics of the penicillin series in tablet forms are identified and quantified by chemometric analysis. The calibration characteristics are linear with approximation reliability coefficients >0.99. The relative standard deviation of the results does not exceed 5%. The analysis time is 15–20 min. [ABSTRACT FROM AUTHOR]

The presence of several minor compounds, such as biophenols, are associated with the quality, health benefits and sensory characteristics of olive oil. The objectives of this study were to compare the profile of the individual phenolic compounds of major brands of olive oils produced in Iran and to correlate the minor polar biophenolic compounds with sensorial properties and finally discriminate the samples. In order to define similarities and differences between Iranian virgin olive oils, profiles of their biophenolic compounds have been investigated using HPLC, analysis of variances and principal component analysis (PCA). Samples of olive oil were notably varied in terms of individual biophenolic compounds and total phenolic content (TPC). Hydroxytyrosol, tyrosol, oleuropein, luteolin, apigenin, and ligstroside aglycone (aldehyde and hydroxylic form) were detected in all samples, whereas caffeic acid was not found in any brands. Based on the differentiating made by PCA, samples were categorized into two distinct groups (TPC300 mg tyrosol/kg of olive oil). The analysis of the main components resulted in a model that describes 86% of the total variance discriminating them from the minor biophenolic compounds of the examined olive oils. This analysis can be considered for assessing the quality and commercial needs related to preferences on olive oil.

The determination of time since death is a major challenge to law enforcement when faced with the discovery of human remains. This is due to the fact that decomposition is a complex, dynamic process influenced by several abiotic and biotic factors. For decades, post-mortem decomposition studies have used pigs as human analogues due to ethical and legal restrictions surrounding the use of human cadavers for such research. However, few comparative studies have been conducted to assess the suitability of these analogues. Recent forensic studies have successfully demonstrated the use of post-mortem lipids in textiles as a method to obtain vital information about decomposition process. The current investigation involved two studies: Trial 1 (summer) and Trial 2 (winter). Each trial with n = 1 human cadaver and n = 2 pigs. Samples were collected over a timeline of 105 days post-placement and analyzed using attenuated total reflectance (ATR-) Fourier-transform infrared (FTIR) spectroscopy. The data was then statistically assessed using functional principal component analysis, semi-parametric regression modeling and analysis of variance. The results demonstrated a clear statistically significant interspecies difference between pigs and humans in both trials. The preliminary implications of this study suggest that pigs are not suitable analogues for humans in decomposition research and have broader implications that caution the direct translation of decomposition data obtained from pigs to real human casework, particularly with respect to time since death estimations.

In this work, an investigation using UHPLC-Q-Orbitrap-MS and multivariate statistics was conducted to obtain the lipid fingerprint of Camembert cheese and to explore its correlated variation with respect to X-ray irradiation treatment. A total of 479 lipids, categorized into 16 different lipid subclasses, were measured. Furthermore, the identification of oxidized lipids was carried out to better understand the possible phenomena of lipid oxidation related to this technological process. The results confirm that the lipidomic approach adopted is effective in implementing the knowledge of the effects of X-ray irradiation on food and evaluating its safety aspects. Furthermore, Partial Least Squares-Discriminant Analysis (PLS-DA) and Linear Discriminant Analysis (LDA) were applied showing high discriminating ability with excellent values of accuracy, specificity and sensitivity. Through the PLS-DA and LDA models, it was possible to select 40 and 24 lipids, respectively, including 3 ceramides (Cer), 1 hexosyl ceramide (HexCer), 1 lysophosphatidylcholine (LPC), 1 lysophosphatidylethanolamine (LPE), 3 phosphatidic acids (PA), 4 phosphatidylcholines (PC), 10 phosphatidylethanolamines (PE), 5 phosphatidylinositols (PI), 2 phosphatidylserines (PS), 3 diacylglycerols (DG) and 9 oxidized triacylglycerols (OxTG) as potential markers of treatment useful in food safety control plans.

Organic biostimulators support wheat growth in unfavorable conditions; however, to date, multifactorial assessments of their role in the plant–pesticide–pathogen system have been poorly investigated. The goal of this study was to evaluate the changes in the metabolite profile (protein, carbohydrate, phenolic compounds, acid phosphatases, and amino acids) and the antioxidant potential (antioxidant enzymes) of wheat that is infested with F. culmorum and exposed to humic acids, nitrophenols, and six pesticides. Additionally, the concentration of the mycotoxins in the wheat grain and the dissipation time of the six pesticides in the wheat plants were determined. In this multifactorial experiment, we explored differentiated activities of humic acids and nitrophenols in wheat metabolism during fungal pathogenesis and pesticide protection. Nitrophenols decreased oxidative stress through induced catalase activity. In contrast, humic acids contributed to the highest enhancement of the total level of carbohydrates (27%) in the inoculated wheat. Both biostimulators reduced the mycotoxin concentration (DON, 3-AcDON, 15-AcDON, NIV) by 32% and nitrophenols increased the concentration of amino acids (13%). Unexpectedly, humic acids and nitrophenols shortened the degradation time (DT50) of spiroxamine by up to 60% in inoculated wheat. The overall results of this study provide novel information on the changes in wheat metabolites, antioxidant defense, and pesticide dissipation in the pesticide–biostimulator–pathogen system.

[Display omitted] • The high consumption of maize requires primarily the identification of transgenic products. • Elemental Spectroscopy techniques provide sufficient information about the samples. • Both non-supervised and supervised multivariate analyses are effective for discrimination. • Internal and external validation provide reliability for classification tasks. In the last decades, the production and consumption of genetically modified agricultural products have increased markedly due to the worldwide population growth and rising demand for food and feed. Consequently, genetically modified crops have been extensively produced and consumed, which required identifying and discriminating transgenic and non-transgenic products. Laser-induced breakdown spectroscopy (LIBS) combined with chemometric methods was applied to identify and discriminate two varieties of conventional (not-genetically modified, NGM) maize from four varieties of transgenic maize (genetically modified, GM). The LIBS spectra acquired under reduced pressure (100 Torr) conditions over two ranges, i.e., 175–330 nm and 275–770 nm, were subjected to Standard Normal Variation (SNV) and multivariate methods such as Principal Component Analysis (PCA) to reduce data matrices dimensionality and spectral noise. The supervised machine learning algorithms k-nearest neighbor (k-NN) and support vector machine (SVM) have been applied to discriminate among NGM and GM maize reserving 25 % of data for external validation. The training data were employed for hyperparameter optimization of classifiers using the Leave-One-Out Cross-Validation (LOOCV) method. Considering all six maize varieties simultaneously, the highest training accuracy achieved was 90.56 %, with an external validation accuracy of 88.33 %. In an alternative approach based on pairwise combinations of one GM variety against one NGM variety, the best outcome achieved was 100 % LOOCV and external validation accuracy. These results showed that LIBS supported by appropriate chemometric methods represents an alternative screening technique for identifying and discriminating transgenic from non-transgenic maize. [ABSTRACT FROM AUTHOR]

Edible oils adulteration has a great concern because of its health and economical effects. Black cumin seed oils (BCSOs) are one of the most adulterated edible oils. In this case, the purpose of this research was to investigate authenticity of commercial BCSOs by spectroscopic and chromatographic techniques combined with orthogonal partial least square-discriminant analysis (OPLS-DA) and hierarchical cluster analysis (HCA). Sixteen commercial BCSO samples (100 % pure-certified and other BCSOs), potential blending oils (sunflower, corn, and soybean oils), and twenty-one synthetically adulterated BCSO samples blended with sunflower (SFO), corn (CO), and soybean (SBO) oils at levels of 5 %, 10 %, 15 %, 20 %, 30 %, 40 %, and 50 % (v/v) were analysed. Screening of potential fingerprinting markers such as thymohydroquinone (THQ), thymoquinone (TQ), carvacrol (CRV), tocopherol isomers (α-, γ-, and δ-), as well as total antioxidant capacity and phenolic content analysis were carried out utilizing spectrophotometric CUPRAC, ABTS, and Folin Ciocalteu's assays. Commercial pure and fraudulent BCSOs and synthetically adulterated samples were successfully classified in OPLS-DA graphs with 95 % confidence level. Even to five percent detection limit for SFO, CO and SBO adulteration were prominently monitored. In consequence, the proposed spectroscopic and chromatographic methods seem to be a practically applicable, sensitive and versatile protocol that can be used as an alternative fingerprinting procedure to determine adulteration of commercial BCSOs. [Display omitted] • Authenticity of commercial black cumin seed oils (BCSOs) was investigated. • Thymoquinone, carvacrol, thymohydroquinone were selected as fingerprinting markers. • Combined spectroscopic and on-line LC analyses of markers were evaluated. • Tocopherol contents and total antioxidant capacities of BCSOs were also examined. • Adulterated BCSOs successfully differentiated from virgin samples using OPLS-DA. [ABSTRACT FROM AUTHOR]

Analysis of vaginal fluid is essential for the diagnosis of cervical cancer, various infections and the increasingly common infertility as well. Surface-enhanced Raman spectroscopy (SERS), which is an ultrasensitive technique, provides information from the molecular level of the analysed system and together with chemometric methods, can be a perfect diagnostic tool. However, the variety of processes naturally occurring during the menstrual cycle has a definite impact on the biochemistry of vaginal swabs. This study adopted SERS to track the biochemical changes recorded in spectra of analysed clinical entities during two menstrual cycles. Using Partial Least Squares Regression (PLSR) technique, we demonstrated the spectral information typical for three types of body fluid: menstrual blood (MB), menstrual spotting (MS) and vaginal fluid (VF). The hormonal changes during the menstrual cycle can be reflected in SERS spectra and allow distinction between the fertile and infertile phases. Significantly larger data separation was observed due to infection rather than hormonal fluctuation. These results give a firm foundation for the diagnosis of vaginal infections regardless of the menstrual cycle's day. • The time-dependent analysis of the menstrual cycle provides the spectral insight into the composition of vaginal secretions. • The SERS-PLSR approach allows effective fertile/infertile phase separation due to changes in circulating biomolecules levels. • An ongoing infection can be recognised by the presence of 730, 1330, 1456 cm-1 bands on the vaginal fluid's SERS spectra. • Vaginal infections lead to a more significant spectral effect than the menstrual cycle does. [ABSTRACT FROM AUTHOR]

Plant-derived bioactive macromolecules (i.e., proteins, lipids, and nucleic acids) were prepared as extracellular vesicles (EVs). Plant-derived EVs are gaining pharmaceutical research interest because of their bioactive components and delivery properties. The spherical nanosized EVs derived from Raphanus sativus L. var. caudatus Alef microgreens previously showed antiproliferative activity in HCT116 colon cancer cells from macromolecular compositions (predominantly proteins). To understand the mechanism of action, the biological activity studies, i.e., antiproliferation, cellular biochemical changes, DNA conformational changes, DNA damage, apoptotic nuclear morphological changes, apoptosis induction, and apoptotic pathways, were determined by neutral red uptake assay, synchrotron radiation-based Fourier transform infrared microspectroscopy, circular dichroism spectroscopy, comet assay, 4′,6-diamidino-2-phenylindole (DAPI) staining, flow cytometry, and caspase activity assay, respectively. EVs inhibited HCT116 cell growth in concentration- and time-dependent manners, with a half-maximal inhibitory concentration of 675.4 ± 33.8 μg/ml at 48 h and a selectivity index of 1.5 ± 0.076. HCT116 treated with EVs mainly changed the cellular biochemical compositions in the nucleic acids and carbohydrates region. The DNA damage caused no changes in DNA conformation. The apoptotic nuclear morphological changes were associated with the increased apoptotic cell population. The apoptotic cell death was induced by both extrinsic and intrinsic pathways. EVs have potential as antiproliferative bioparticles. [Display omitted] • Extracellular vesicles (EVs) were released from R. sativus var. caudatus microgreens. • EVs comprised bioactive macromolecules with predominant β-pleated sheet proteins. • HCT116 cellular biochemical changed, especially nucleic acids, after EV treatment. • HCT116 apoptotic cell death was caused by DNA damage after EV treatment. • HCT116 death was via both intrinsic and extrinsic apoptotic pathway induction by EVs. [ABSTRACT FROM AUTHOR]

• Katsuobushi characterized by FTIR, NIR, and GC–MS for smoking treatments. • PCA, PLS-DA, and HCA correctly classified katsuobushi by smoking treatment. • Multivariate analysis showed UV–Vis-NIR's greater efficacy than FTIR. • An accurate quality prediction model was built through PLSR analysis. • It is feasible to estimate Katsuobushi quality based on the FTIR and NIR spectra. Katsuobushi, a smoked, dried skipjack tuna, is a traditional Japanese food additive with a unique flavor and taste. Gas chromatography mass spectrometry (GC-MS), fourier transform infrared (FTIR), and ultraviolet-visible-near infrared spectroscopy (UV-Vis-NIR) combined with chemometric methods were evaluated the quality of katsuobushi according to the number of smoking treatments. Using GC-MS, 46 metabolites were identified and five metabolites were selected as key compounds. All samples were classified according to their smoking number via principal component analysis (PCA), partial least squares-discriminate analysis (PLS-DA) and hierarchical cluster analysis (HCA) of the FTIR and NIR spectra. Partial least squares regression (PLSR) analysis revealed that the FTIR and NIR spectra were highly correlated with the metabolites by GC-MS. These results demonstrated the potential of using the FTIR and NIR spectroscopy combined with chemometrics to assess the quality of katsuobushi based on the smoking treatments, with NIR spectroscopy showed particularly promising. [ABSTRACT FROM AUTHOR]

The chemical composition of the essential oils (EOs) of Stachys byzantina, S. hissarica and S. betoniciflora growing in Uzbekistan were determined, and their antioxidant and enzyme inhibitory activity were assessed. A gas chromatography-mass spectrometry (GC-MS) analysis revealed the presence of 143 metabolites accounting for 70.34, 76.78 and 88.63% of the total identified components of S. byzantina, S. hissarica and S. betoniciflora, respectively. Octadecanal (9.37%) was the most predominant in S. betoniciflora. However, n-butyl octadecenoate (4.92%) was the major volatile in S. byzantina. Benzaldehyde (5.01%) was present at a higher percentage in S. hissarica. A chemometric analysis revealed the ability of volatile profiling to discriminate between the studied Stachys species. The principal component analysis plot displayed a clear diversity of Stachys species where the octadecanal and benzaldehyde were the main discriminating markers. The antioxidant activity was evaluated in vitro using 2,2-diphenyl-1-picryl-hydrazyl (DPPH), 2,2-azino bis (3-ethylbenzothiazoline-6-sulphonic acid) (ABTS), cupric reducing antioxidant capacity (CUPRAC), ferric reducing power (FRAP), chelating and phosphomolybdenum (PBD). Moreover, the ability of the essential oils to inhibit both acetyl/butyrylcholinesterases (AChE and BChE), α-amylase, α-glucosidase and tyrosinase was assessed. The volatiles from S. hissarica exhibited the highest activity in both the ABTS (226.48 ± 1.75 mg Trolox equivalent (TE)/g oil) and FRAP (109.55 ± 3.24 mg TE/g oil) assays. However, S. betoniciflora displayed the strongest activity in the other assays (174.94 ± 0.20 mg TE/g oil for CUPRAC, 60.11 ± 0.36 mg EDTA equivalent (EDTAE)/g oil for chelating and 28.24 ± 1.00 (mmol TE/g oil) for PBD. Regarding the enzyme inhibitory activity, S. byzantina demonstrated the strongest AChE (5.64 ± 0.04 mg galantamine equivalent (GALAE)/g oil) and tyrosinase inhibitory (101.07 ± 0.60 mg kojic acid equivalent (KAE)/g) activity. The highest activity for BChE (11.18 ± 0.19 mg GALAE/g oil), amylase inhibition (0.76 ± 0.02 mmol acarbose equivalent (ACAE)/g oil) and glucosidase inhibition (24.11 ± 0.06 mmol ACAE/g oil) was observed in S. betoniciflora. These results showed that EOs of Stachys species could be used as antioxidant, hypoglycemic and skincare agents. [ABSTRACT FROM AUTHOR]

Cannabis sativa L. is an annual herbaceous plant that belongs to the family Cannabinaceae. In this study, the potential use of forty-five cannabinoids, previously identified from Cannabis sativa to alleviate COVID-19 infection via prohibition of crucial SARS-CoV-2 proteins using molecular docking, was examined. In silico studies were performed on three vital enzymes that serve as principle therapeutic targets to prevent SARS-CoV-2 replication. These enzymes are the main protease SARS-CoV-2 MPro, papain-like protease SARS-CoV-2 PLpro and angiotensin-converting enzyme 2 (ACE2). Regarding SARS-CoV-2 MPro, cannabichromanon (32) showed the best fitting within its active centers, followed by cannabinolic acid (22) and cannabinol (21), displaying ∆G of −33.63, −23.24, and −21.60 kcal/mol, respectively. Concerning SARS-CoV-2 PLpro, cannabichromanon (32) followed by cannabinolic acid (22) and cannabicyclolic acid (41) revealed the best binding within its active pockets owing to multiple bond formation with ∆G values of −28.36, −22.81, and −19.89 kcal/mol. Furthermore, cannabichromanon (32), cannabinolic acid (22), and cannabinol (21) showed considerable fitting within the active sites of angiotensin-converting enzyme 2 (ACE2) evidenced by their significant ∆G values that were estimated as −41.77, −31.34, and −30.36 kcal/mol, respectively. ADME/TOPKAT (absorption, distribution, metabolism, excretion, and toxicity) evaluation was performed on the tested cannabinoids to further explore their pharmacokinetics, pharmacodynamics, and toxicity properties. The results indicated the considerable pharmacokinetic, pharmacodynamic, and toxicity properties of cannabinol (21), cannabinolic acid (22), cannabichromanon (32), and cannabicyclolic acid (41) that showed best fitting scores within the active sites of the tested enzymes. Multivariate data analysis revealed that cannabichromanon and cannabinolic acid showed a discriminant nature and hence can be incorporated in pharmaceutical dosage forms to alleviate COVID-19 infection. [ABSTRACT FROM AUTHOR]

Oil samples from the Halfaya, Noor, and Amara oilfields were geochemically characterized to determine their origin, type of organic matter, and the depositional environment conditions of the correlative source rocks. Detailed saturated and aromatic biomarkers from nine oil samples were analyzed using gas chromatography and gas chromatography-mass spectrometry, and measurement of sulfur content and stable carbon isotopes. Saturated hydrocarbons in the oil samples are low, whereas polar fractions are relatively high. Saturated (terpane and sterane) and aromatic biomarker ratios suggest that these oil samples were generated mainly from early to mid-mature carbonate source rocks. The anoxic marine depositional environment of the source rocks is reflected by the high C35S/C34S hopane and low Pr/Ph ratios. Hierarchical cluster analysis (HCA) identifies two oil families. These oil families may have originated from the same source rock but with different organofacies. Regular sterane distributions differ from those for oils from the southern oilfields (Majnoon, Nasiriah, West Qurna, North Rumaila, Luhais, Abu Gharab, Faka, Buzergan). Biomarker ratios indicate that the present study oils are slightly more mature than southern oils and their source rock depositional environment was more reducing (anoxic). Based on comparison with previously published data, the most likely source rocks for the present study oils include the Sulaiy, Yamama, and Zubair formations. [ABSTRACT FROM AUTHOR]

Plant growth and survival in nature, its growth process, will be affected by various factors from the environment, among which temperature has a greater impact. In recent years, extreme weather has frequently appeared, and the growth of crops has been increasingly affected by the environment. As an important flavoring and Chinese herbal medicine crop, Zanthoxylum bungeanum is also facing the harm of low-temperature stress. Plant hormones play a vital role in the response of plants to low temperatures. In this study, ultra-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used to determine the hormone components of cold-tolerant and cold-sensitive varieties of Z. bungeanum. Combined with chemometric analysis and weighted gene co-expression network analysis (WGCNA), the hormone component differences and hormone response strategies of Z. bungeanum under low-temperature stress were comprehensively studied. The results showed that 45 hormones were detected in Z. bungeanum. Among them, there were 7 kinds of components with high content and were detected in both two varieties. At the late stage of low-temperature stress, the contents of abscisic acid (ABA) and ABA-glucosyl ester (ABA-GE) in Fuguhuajiao (FG) were significantly increased, and the latter served as the storage of the former to supplement the active ABA. Orthogonal partial least squares discriminant analysis (OPLS-DA) found that indole-3-carboxylic acid (ICA), indole-3-carboxaldehyde (ICAld), meta-Topolin riboside (mTR), cis-Zeatin-O-glucoside riboside (cZROG), and N6-isopentenyladenosine (IPR) in FG were the upregulated important difference components, and IPR and 2-methylthio-cis-zeatin riboside (2MeScZR) in Fengxiandahongpao (FX) were the upregulated important difference components. There were common crossing points and independent response pathways in response to low temperature in two varieties. WGCNA analysis found that the main hormone components were associated with multiple metabolic pathways including carbon, fatty acid, amino acid, and sugar metabolism, indicating that hormone regulation plays an important role in the response of Z. bungeanum to low temperature. This study clarified the hormone response mechanism of Z. bungeanum under low-temperature stress and provided a reference and basis for further improving the cold resistance of Z. bungeanum and cultivating new varieties. [ABSTRACT FROM AUTHOR]

The objective of this study is to develop a statistical model to accurately estimate the total base number (TBN) value of diesel engine oils on the basis of the Fourier transform infrared spectroscopy (FTIR) analysis. The research sample consisted of oils used in the course of 14,820 km. The samples were collected after each 1000 km and both FTIR and TBN measurements were performed. By applying the measured absorbance values, five statistical models aimed at predicting TBN values were elaborated with the use of the following information: aggregated values of measured absorbance in defined spectral ranges, extremes at wavenumbers, or the surface area of spectral bands related to the vibrations of specific molecular structures. The obtained models may be considered a continuation and an extension of previous studies of this type described in the literature on the subject. The results of the study and the analysis of the obtained data have led to the development of two models with high predictive capabilities (R2 > 0.98, RMSE < 0.5). Another model, which had the smallest number of variables in comparison to other models, had markedly lower R2 value (0.9496) and the highest RMSE (0.5596). Yet another model, where the dimensionality of the pre-processed full spectra was reduced to four aggregates through averaging, turned out to be slightly worse than the best one (R2 = 0.9728). The study contributes to a more in-depth understanding of the FTIR-based TBN prediction tools that may be readily available to all interested parties. [ABSTRACT FROM AUTHOR]

Label-free molecular imaging is a promising utility to study tissues in terms of the identification of their compartments as well as chemical features and alterations induced by disease. The aim of this work was to assess if higher magnification of optics in the Fourier transform infrared (FT-IR) microscope coupled with the focal plane detector resulted in better resolution of lung structures and if the histopathological features correlated with clustering of spectral images. FT-IR spectroscopic imaging was performed on paraffinized lung tissue sections from mice with optics providing a total magnification of 61× and 36×. Then, IR images were subjected to unsupervised cluster analysis and, subsequently, cluster maps were compared with hematoxylin and eosin staining of the same tissue section. Based on these results, we observed minute features such as cellular compartments in single alveoli and bronchiole, blood cells and megakaryocytes in a vessel as well as atelectasis of the lung. In the case of the latter, differences in composition were also noted between the tissue from the non-cancerous and cancerous specimen. This study demonstrated the ability of high-definition FT-IR imaging to evaluate the chemical features of well-resolved lung structures that could complement the histological examination widely used in animal models of disease. Graphical Abstract [ABSTRACT FROM AUTHOR]

BACKGROUND Zanthoxylum bungeanum pericarps (ZBP) are commonly used as food additives and traditional herbal medicines. Several mineral elements are known to have important physiological functions in organisms, whereas others are reported to have toxic effects. We determined levels of macro elements (Mg, S and Ca), essential trace elements (B, Mn, Fe, Cu, Zn, Se and Mo) and toxic elements (Ni, Al, Cr, As, Cd, Hg and Pb) in the pericarps of 19 Z. bungeanum cultivars. Hazard index values and incremental lifetime cancer risks were calculated to express health risks associated with pericarp consumption. Moreover, several chemometric analyses based on the mineral elements were used to distinguish Z. bungeanum cultivars. RESULTS: The concentrations of 17 determined elements in the pericarps were ranked: Ca > Mg > S > Fe > Al > Mn > Zn > B > Cu > Ni > Pb > Cr > Mo > As > Cd > Hg > Se. The elements Zn, Cr and As had the highest variations in their concentrations. Cu, Mn, Se, Zn, Al, As, Cd, Cr, Hg, Ni and Pb posed some non‐cancer risks, while As and Cd posed cancer risks. Mn, Fe, Zn, and Al were chosen as critical element markers for assessing ZBP using chemometric analyses. CONCLUSION: Chemometric analyses could highlight mineral concentration differentiation among the 19 cultivars. The Z. bungeanum cultivar Z12 (from Wudu, Gansu) is best for producing ZBP, and cultivar Z18 (Guanling, Guizhou) can be a reference to classify and evaluate ZBP quality. The results provide valuable information for evaluating the potential safety risks of ZBP and contribute to inter‐cultivar discrimination. © 2021 Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

A combined approach was developed for the identification and determination of quinolone antibiotics in pharmaceuticals using solid-state fluorescence digital colorimetry and chemometric analysis. The eigen fluorescence of quinolones and quinolone-sensitized fluorescence of europium(III) were studied in various matrices. A test system consisting of four indicator zones was proposed. Irradiation by UV light (365 nm) of quinolone solutions applied to the indicator zones of test systems produced blue fluorescence on cellulose paper (CP) and plates for high-performance thin layer chromatography (HPTLC) and pink fluorescence (CP–Eu, HPTLC–Eu). The fluorescence intensity on the surface of the matrices was measured using a smartphone. It was shown that chemometric analysis, which enabled the analysis time to be reduced and research data to be visualized, could be used. The data were processed by principal component analysis (PCA), hierarchical cluster analysis, and the k-means method using XLSTAT software. Quinolone antibiotics in tablet forms were identified and quantified using chemometric analysis. Calibration curves in the PCA and k-means methods had a logarithmic form in the determined concentration range of 0.5–250 μg/mL (R2 ≥ 0.98). A technique for determination of fluoroquinolones in pharmaceuticals was proposed. The relative standard deviation did not exceed 0.09. [ABSTRACT FROM AUTHOR]

Introduction: Morus alba L. is one of the economic plants in Thailand. Several varieties are grown in various parts of the country. Different varieties from different regions may produce dissimilar chemical fingerprints. Objectives: The gas chromatography coupled to mass spectrometry (GC-MS) fingerprints of 2 varieties of M. alba leaves from three locations in Thailand, along with tea products will be established. Materials and Methods: The GC-MS chromatograms combined with chemometric analysis were used to analyze the extracts of M. alba leaves and their tea products. Results: A total of 83 compounds comprising terpenes, saturated fatty acids, unsaturated fatty acids and benzofurans were found in M. alba leaves from both varieties. Fifteen compounds such as phytol, oleic acid, and palmitic acid, with % peak area (detected at >0.04%) from high to low, were found in var. Buriram 60. Eighteen compounds such as phytol, palmitic acid, and oleic acid, respectively, were found in var. Khun Pai. Six compounds, that is, methyl palmitate, palmitic acid, methyl linolenate, phytol, oleic acid, and stearic acid were found in the tea products. Conclusion: The GC-MS fingerprints were combined with chemometric analysis for the authentication and characterization of two varieties of M. alba leaves from Thailand. [ABSTRACT FROM AUTHOR]

A urine-based screening technique for Lyme disease (LD) was developed in this research. The screen is based on Raman spectroscopy, iterative smoothing-splines with root error adjustment (ISREA) spectral baselining, and chemometric analysis using Rametrix software. Raman spectra of urine from 30 patients with positive serologic tests (including the US Centers for Disease Control [CDC] two-tier standard) for LD were compared against subsets of our database of urine spectra from 235 healthy human volunteers, 362 end-stage kidney disease (ESKD) patients, and 17 patients with active or remissive bladder cancer (BCA). We found statistical differences (p < 0.001) between urine scans of healthy volunteers and LD-positive patients. We also found a unique LD molecular signature in urine involving 112 Raman shifts (31 major Raman shifts) with significant differences from urine of healthy individuals. We were able to distinguish the LD molecular signature as statistically different (p < 0.001) from the molecular signatures of ESKD and BCA. When comparing LD-positive patients against healthy volunteers, the Rametrix-based urine screen performed with 86.7% for overall accuracy, sensitivity, specificity, positive predictive value (PPV), and negative predictive value (NPV), respectively. When considering patients with ESKD and BCA in the LD-negative group, these values were 88.7% (accuracy), 83.3% (sensitivity), 91.0% (specificity), 80.7% (PPV), and 92.4% (NPV). Additional advantages to the Raman-based urine screen include that it is rapid (minutes per analysis), is minimally invasive, requires no chemical labeling, uses a low-profile, off-the-shelf spectrometer, and is inexpensive relative to other available LD tests. Graphical Abstract [ABSTRACT FROM AUTHOR]

Hematuria refers to the presence of blood in urine. Even in small amounts, it may be indicative of disease, ranging from urinary tract infection to cancer. Here, Raman spectroscopy was used to detect and quantify macro- and microhematuria in human urine samples. Anticoagulated whole blood was mixed with freshly collected urine to achieve concentrations of 0, 0.25, 0.5, 1, 2, 6, 10, and 20% blood/urine (v/v). Raman spectra were obtained at 785 nm and data analyzed using chemometric methods and statistical tests with the Rametrix toolboxes for Matlab. Goldindec and iterative smoothing splines with root error adjustment (ISREA) baselining algorithms were used in processing and normalization of Raman spectra. Rametrix was used to apply principal component analysis (PCA), develop discriminate analysis of principal component (DAPC) models, and to validate these models using external leave-one-out cross-validation (LOOCV). Discriminate analysis of principal component models were capable of detecting various levels of microhematuria in unknown urine samples, with prediction accuracies of 91% (using Goldindec spectral baselining) and 94% (using ISREA baselining). Partial least squares regression (PLSR) was then used to estimate/quantify the amount of blood (v/v) in a urine sample, based on its Raman spectrum. Comparing actual and predicted (from Raman spectral computations) hematuria levels, a coefficient of determination (R2) of 0.91 was obtained over all hematuria levels (0–20% v/v), and an R2 of 0.92 was obtained for microhematuria (0–1% v/v) specifically. Overall, the results of this preliminary study suggest that Raman spectroscopy and chemometric analyses can be used to detect and quantify macro- and microhematuria in unprocessed, clinically relevant urine specimens. [ABSTRACT FROM AUTHOR]

Monitoring and assessment of soil quality are important in mining areas. In this study, indexical, spatiotemporal, and chemometric models were developed to monitor and assess the pollution level and health risk of potentially toxic elements (PTEs) within the Iyamitet-Okurumutet mine province, SE Nigeria. Surface soils were sampled within the mine area and analyzed for pH, cation exchange capacity, organic matter, and PTEs (Pb, Zn, Cd, Mn, Fe, Ba) following standard techniques. It was revealed that the soils are slightly acidic and the enrichment of PTEs except for Cd (4.08 mg/kg−1) was within recommended standards. Contamination factor, enrichment factor, and pollution index suggest that the soils are moderately polluted. Geospatial maps and ecological risk indices revealed that higher ecological risk imprints seem to increase towards the south-eastern parts of the area. Chemometric analysis revealed that PTE enrichment in the soil is majorly influenced by anthropogenic activities. Further, bioavailability/bioaccessibility risk assessment index (BRAI) and health risk assessment models were developed to quantify the bioavailable/human bioaccessible portion of elements in soils and the associated health risks. The BRAI ranged from high (3 ≥ 5) to very high (> 5) risk of human bioaccessibility; hence, greater amount of PTEs will be bioaccessible for absorption into the human gastrointestinal system than they would for plants uptake. The hazard index and lifetime cancer risk (LCR) revealed that most of the samples present high chronic cancer risks from dermal contact and ingestion for children and adults. The LCR values ranged between 1.0E-6 and 1.0E − 04, with the children population showing greater vulnerability to cancer risks. [ABSTRACT FROM AUTHOR]

Introduction: Praxelis genus comprises 24 species, however, only two species of this genus have been chemically investigated. Here we investigated Praxelis sanctopaulensis, a native plant from Brazil, that occurs mainly in Cerrado regions. Objective: The goal was to identify the specialised metabolites from P. sanctopaulensis, and compare with those described from Praxelis and Chromolaena species. Methods: The phytochemical study of P. sanctopaulensis was performed through different chromatography techniques, including high‐performance liquid chromatography (HPLC), gas chromatography flame ionisation detector (GC‐FID), and ultra‐high‐performance liquid chromatography high‐resolution tandem mass spectrometry (UHPLC‐HRMS/MS). The structures of the compounds were established based on spectroscopic analysis, total correlated spectroscopy (TOCSY), hydrogen decoupling and computational calculations was used to an unequivocal structural elucidation of a new sesquiterpene. The antioxidant activity was evaluated using 1,1‐diphenyl‐2‐picrylhydrazyl (DPPH) and ferric reducing antioxidant power (FRAP), and antimicrobial assay was performed by the microdilution method. Comparison of the flavonoids described P. sanctopaulensis was carried out using principal component analysis. Results: The phytochemical investigation of P. sanctopaulensis led to the isolation of a pair of diastereomers, praxilone A and praxilone B. Seven known compounds were isolated from this species, another 14 fatty acids were detected in hexane fraction, and 26 compounds were identified from ethyl acetate fraction. All these compounds are being described for the first time in this species, with the exception of viridifloric acid. The ethyl acetate fraction showed potent antioxidant activity. Conclusions: Forty‐seven compounds are described from P. sanctopaulensis. The combination of different techniques of nuclear magnetic resonance (NMR) spectroscopy and computational calculations allowed the unequivocal structure elucidation of a new cadinene. The clustering analysis showed similarities between the flavonoids identified in P. sanctopaulensis and in Chromolaena species. Forty‐seven compounds are being described from P. sanctopaulensis, using classical phytochemistry and dereplication techniques. The combination of different techniques of NMR spectroscopy and computational calculations allowed the unequivocal structure elucidation of a new cadinene, this compound was isolated as a pair of diastereomers. All these compounds are being described for the first time in Praxelis genus, with exception of viridifloric acid, showing the relevance of this work for the chemical knowledge of Asteraceae species. [ABSTRACT FROM AUTHOR]

The food products may attract unscrupulous vendors to dilute it with inexpensive alternative food sources to achieve more profit. The risk of high value food adulteration with cheaper substitutes has reached an alarming stage in recent years. Commonly available detection methods for food adulteration are costly, time consuming and requires high degree of technical expertise. However, a rapid and suitable detection method for possible adulterant is being evolved to tackle the aforesaid issues. In recent years, electronic nose (e-nose) system is being evolved for falsification detection of food products with reliable and rapid way. E-nose has the ability to artificially perceive aroma and distinguish them. The use of chemometric analysis together with gas sensor arrays have shown to be a significant procedure for quality monitoring in food. E-nose techniques with numerous provisions are reliable and favourable for food industry in food fraud detection. In the present review, the contributions of gas sensor based e-nose system are discussed extensively with a view to ascertain the adulteration of food products. [ABSTRACT FROM AUTHOR]

Preterm newborns are extremely vulnerable to morbidities, complications, and death. Preterm birth is a global public health problem due to its socioeconomic burden. Nurturing preterm newborns is a critical medical issue because they have limited nutrient stores and it is difficult to establish enteral feeding, which leads to inadequate growth frequently associated with poor neurodevelopmental outcomes. Parenteral nutrition (PN) provides nutrients to preterm newborns, but its biochemical effects are not completely known. To study the effect of PN treatment on preterm newborns, an untargeted metabolomic 1H nuclear magnetic resonance (NMR) assay was performed on 107 urine samples from 34 hospitalized patients. Multivariate data (Principal Component Analysis, PCA, Orthogonal partial least squares discriminant analysis OPLS-DA, parallel factor analysis PARAFAC-2) and univariate analyses were used to identify the association of specific spectral data with different nutritional types (NTs) and gestational ages. Our results revealed changes in the metabolic profile related to the NT, with the tricarboxylic acid cycle and galactose metabolic pathways being the most impacted pathways. Low citrate and succinate levels, despite higher glucose relative urinary concentrations, seem to constitute the metabolic profile found in the studied critically ill preterm newborns who received PN, indicating an energetic dysfunction that must be taken into account for better nutritional management. [ABSTRACT FROM AUTHOR]

Milk-based kombucha beverages were obtained conducting kombucha lead fermentation of milk. In order to discriminate the analysed samples and to detect similarities or dissimilarities among them in the space of experimentally determined variables, hierarchical cluster analysis (HCA) and principal component analysis (PCA) were applied. Linear discriminant analysis (LDA) was conducted on the raw data set in order to find a rule for allocating a new sample of unknown origin to the correct group of samples. In the space of the variables analysed by HCA, the dominant discriminating factor for the studied samples of kombucha beverages is the milk fat (MF) content, followed by total unsaturated fatty acids content (TUFA), monounsaturated fatty acids content (MUFA) and polyunsaturated fatty acids content (PUFA). The samples with 0.8 and 1.6% milk fat belong to the same cluster in the space of the analysed variables due to similarities in their AADPPH. It was determined by LDA that there was the biggest difference in quality between the groups of products with winter savoury and stinging nettle, while the highest similarity is between groups of products with wild thyme and peppermint regarding their pH values and antioxidant activity expressed as AADPPH.

Monk fruit, also named Luo Han Guo, is the fruit of Siraitia grosvenorii (Swingle) C. Jeffrey ex A. M. Lu et Z. Y. Zhang and has been used as both food and traditional Chinese medicine. Due to preservation concerns, monk fruit is usually processed by hot-air drying or using low-temperature techniques after harvest. In this study, high-performance thin-layer chromatography (HPTLC) method was developed for the analysis of 13 mogrosides, 1 flavonoid, and 3 sugars in monk fruit products. Then chemometric analysis was applied to investigate the chemical characteristics in the samples dried by different methods. The results showed that the contents of mogroside V, 11-oxo-mogroside V, isomogroside V, and sucrose in monk fruits dried at low temperature were much higher than those in traditional hot-air drying samples, which was also confirmed by HPTLC-scanning. These findings indicate that HPTLC combined with chemometric analysis provides a reliable tool to understand the chemical differences between the monk fruit products processed by different drying methods, which will be helpful for their quality evaluation.

Plant growth and survival in nature, its growth process, will be affected by various factors from the environment, among which temperature has a greater impact. In recent years, extreme weather has frequently appeared, and the growth of crops has been increasingly affected by the environment. As an important flavoring and Chinese herbal medicine crop, Zanthoxylum bungeanum is also facing the harm of low-temperature stress. Plant hormones play a vital role in the response of plants to low temperatures. In this study, ultra-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used to determine the hormone components of cold-tolerant and cold-sensitive varieties of Z. bungeanum. Combined with chemometric analysis and weighted gene co-expression network analysis (WGCNA), the hormone component differences and hormone response strategies of Z. bungeanum under low-temperature stress were comprehensively studied. The results showed that 45 hormones were detected in Z. bungeanum. Among them, there were 7 kinds of components with high content and were detected in both two varieties. At the late stage of low-temperature stress, the contents of abscisic acid (ABA) and ABA-glucosyl ester (ABA-GE) in Fuguhuajiao (FG) were significantly increased, and the latter served as the storage of the former to supplement the active ABA. Orthogonal partial least squares discriminant analysis (OPLS-DA) found that indole-3-carboxylic acid (ICA), indole-3-carboxaldehyde (ICAld), meta-Topolin riboside (mTR), cis-Zeatin-O-glucoside riboside (cZROG), and N6-isopentenyladenosine (IPR) in FG were the upregulated important difference components, and IPR and 2-methylthio-cis-zeatin riboside (2MeScZR) in Fengxiandahongpao (FX) were the upregulated important difference components. There were common crossing points and independent response pathways in response to low temperature in two varieties. WGCNA analysis found that the main hormone components were associated with multiple metabolic pathways including carbon, fatty acid, amino acid, and sugar metabolism, indicating that hormone regulation plays an important role in the response of Z. bungeanum to low temperature. This study clarified the hormone response mechanism of Z. bungeanum under low-temperature stress and provided a reference and basis for further improving the cold resistance of Z. bungeanum and cultivating new varieties.

Ion mobility (IM) is an important analytical technique for determining ion collision cross section (CCS) values in the gas-phase and gaining insight into molecular structures and conformations. However, limited instrument resolving powers for IM may restrict adequate characterization of conformationally similar ions, such as structural isomers, and reduce the accuracy of IM-based CCS calculations. Recently, we introduced an automated technique for extracting pure IM and collision-induced dissociation (CID) mass spectra of IM overlapping species using chemometric deconvolution of post-IM/CID mass spectrometry (MS) data [J. Am. Soc. Mass Spectrom., 2014, 25, 1810-1819]. Here we extend those capabilities to demonstrate how extracted IM profiles can be used to calculate accurate CCS values of peptide isomer ions which are not fully resolved by IM. We show that CCS values obtained from deconvoluted IM spectra match with CCS values measured from the individually analyzed corresponding peptides on uniform field IM instrumentation. We introduce an approach that utilizes experimentally determined IM arrival time (AT) shift factors to compensate for ion acceleration variations during post-IM/CID and significantly improve the accuracy of the calculated CCS values. Also, we discuss details of this IM deconvolution approach and compare empirical CCS values from traveling wave (TW)IM-MS and drift tube (DT)IM-MS with theoretically calculated CCS values using the projected superposition approximation (PSA). For example, experimentally measured deconvoluted TWIM-MS mean CCS values for doubly-protonated RYGGFM, RMFGYG, MFRYGG, and FRMYGG peptide isomers were 288.8 Å(2), 295.1 Å(2), 296.8 Å(2), and 300.1 Å(2); all four of these CCS values were within 1.5% of independently measured DTIM-MS values.

Optical spectroscopy is a powerful characterization tool with applications ranging from fundamental studies to real-time process monitoring. However, it can be difficult to apply to complex samples that contain interfering analytes which are common in processing streams. Multivariate (chemometric) analysis has been examined for providing selectivity and accuracy to the analysis of optical spectra and expanding its potential applications. Here we will discuss chemometric modeling with an in-depth comparison to more simplistic analysis approaches and outline how chemometric modeling works while exploring the limits on modeling accuracy. Understanding the limitations of the chemometric model can provide better analytical assessment regarding the accuracy and precision of the analytical result. This will be explored in the context of UV–Vis absorbance of neodymium (Nd3+) in the presence of interferents, erbium (Er3+) and copper (Cu2+) under conditions simulating the liquid–liquid extraction approach used to recycle plutonium (Pu) and uranium (U) in used nuclear fuel worldwide. The selected chemometric model, partial least squares regression, accurately quantifies Nd3+ with a low percentage error in the presence of interfering analytes and even under conditions that the training set does not describe. Graphical Abstract [ABSTRACT FROM AUTHOR]

Genus Lavandula belongs to Lamiaceae family containing almost 40 different species, many hybrids, and nearly 400 registered cultivars (Upson and Andrews 2004). Mane folk uses and biological activities of Lavandula species are reported in addition to their uses in the pharmaceutical and other industries benefits. The biological activities of Lavandula leaves are usually correlated to the essential oils (EOs) and volatiles that represented the main constituents of the leaves. Many compounds were identified and characterized in the extracted EOs from Lavandula leaves around the world. Chemical polymorphism is a phenomenon where the same species showed variation in the chemical composition of the bioactive compounds. This phenomenon is well known for the EOs of various plants. Therefore, the present work aimed for chemical profiling of three EOs isolated from the leaves of Lavandula species grown in Egypt (L. angustifolia, Lavandula x intermedia or L. hybrid and L. spica) and other three from French and Australia (L. angustifolia and L. latifolia from Australia and L. stoechas L. from French). In addition, established the chemical based relationship among the five species using chemometric analysis. The qualitative and quantitative analyses of the main constituents of the EOs were studied. A total of 74 volatile compounds were identified from the aerial parts of L. angustifolia, L. latifolia from Australia and L. stoechas from French and lavandin (Lavandula hybrida), L. angustifolia and L. spica cultivated in Egypt, representing 99.87, 98.94, 98.93, 98.89, 99.89 and 99.28% of the total mass, respectively. The identified compound classes were characterized as mono-, sesqui- oxygenated and non-oxygenated terpenoids. The main constituents in the different species were linalool (39.5%), lianlyl acetate (26.7%), eucalyptol (43.08%), tau-cadinol (28.63%), linalyl acetate (46.41%) and tau-cadinol (19.08%) for AUS Lavander, Fren. lavnder, lavandin, L. angistifolia, L. latifolia, and L. asp, respectively. Major components analysis showed that there is significant variation between species in the quality and quantity of EO composition. All lavandula species/varieties appeared to be richest in oxygenated monoterpenes. These major compounds have been reported as biologically effective compounds with various activities. The characterization of chemotypes in cultivated plants is crucial for agriculture application, chemistry purposes, and pharmacological uses. [ABSTRACT FROM AUTHOR]

The study aimed to evaluate fourteen elements' profiles of legumes and oilseeds, of various geographical origins, available on the Polish market. They were determined by flame atomic absorption spectrometry (F-AAS) and spectrophotometric method (phosphorus) in 90 analytical samples. In general, legumes were characterized with lower mean concentrations of Ca, Mg, Na, P, Zn, Cu, Fe, Mn, and Cr than oilseeds. However, the concentrations ranges within each group differed significantly (p < 0.05). Calcium content varied between 6.2 and 243.5 mg/100 g in legumes and 38.4 and 2003 mg/100 g in oilseeds. In the case of Fe, its concentration was between 1.99 mg/100 g and 10.5 mg/100 g in legumes, and 2.05 mg and 12.15 mg/100 g in seeds. All the samples were characterized with Pb concentration below the LOQ (30 µg/100 g). In the case of Cd, its presence (>LOQ, 9 µg/100 g) was confirmed in one sample of legumes (soybean) and five samples of seeds (poppy seeds, roasted linseeds, hulled wheat, linseed, and sunflower seeds). The detected Cd content in every sample, except for soybean and hulled wheat, exceeded the permissible European standards. According to Kruskal-Wallis test results, Mg, Na, K, P, Zn, Cu, Mn, Cr, and Cd content depended on the type of the analyzed product, while in the case of botanical provenance such relationship was recorded for most of the analyzed components, except for Fe, Cr, and Co. Factor and cluster analyses classified the analyzed samples in view of their botanical species and type based on their mineral composition. [ABSTRACT FROM AUTHOR]

Validated HPLC and UV analysis were applied for quantitative determination of six isoflavones (daidzin, glycitin, genistin, daidzein, glycitein, and genistein) in soy products. In HPLC analysis, six isoflavones showed satisfactory regression (r2 > 0.99) within test ranges, and the recovery was in the range of 91.00 to 117.00%. LOD and LOQ ranged from 0.004–0.016 (µg ml−1) and 0.015–0.035 (µg ml−1), respectively. The quantified isoflavones present in prepared and commercial extracts were then subjected to principal component analysis (PCA), in conjunction with hierarchical cluster analysis (HCA), which showed differences in the isoflavone from soybeans. The employment of a simple and low-cost UV spectrophotometric methodology was also applied in quantification of same compounds in the same soy extracts. Paired t-test confirmed that there is no significant difference between the results obtained for the two methods. Our results revealed that the developed methods have potential perspective for the original discrimination and quality control of isoflavones in soybean-based products employing a rapid, fast, and not-expensive method. [ABSTRACT FROM AUTHOR]

The objective of this study was provide the first report to assess the high-performance liquid chromatography-diode array detection (HPLC-DAD) identification of phytochemicals, the spectrophotometric determination of total phenolics and flavonoids, and antioxidant activities of the root and aerial extracts of Chaerophyllum bulbosum. HPLC-DAD identified the main phytochemical to be rosmarinic acid in the roots in the acetone (CBRA) (13.98 ± 0.12 mg/g) and the aerial water (CBAW) extract; myricetin (8.30 ± 0.22 mg/g) in the root methanol extract (CBRM); trans-aconitic acid (6.46 ± 0.49 mg/g) in the root water extract (CBRW) and fumaric acid in the aerial methanol (CBAM) (17.43 ± 0.87 mg/g) and water CBAW (18.96 ± 0.81 mg/g) extracts. The concentrations of total phenolics and flavonoids were 2.00 ± 0.14-17.79 ± 0.99 µg PEs/mg extract and 2.90 ± 0.00-27.64 ± 0.37 µg QEs/mg extract, respectively. The highest antioxidant activity was found in the root acetone extract (CBRA) using the β-carotene-linoleic (IC50: 172.31 ± 0.16 µg/mL) and CUPRAC (A0.50: 126.00 ± 0.24 µg/mL) assays and in the root water extract (CBRW) for DPPH• (IC50: 59.51 ± 0.21 µg/mL) and metal chelating (IC50: 65.91 ± 0.36 µg/mL) assays in the aerial water extract (CBAW) using the ABTS•+ (IC50: 59.51 ± 0.21 µg/mL) assay. The relationship between the phytochemicals and antioxidant activities of the extracts was chemometrically determined by principal component analysis (PCA) and hierarchical cluster analysis (HCA). [ABSTRACT FROM AUTHOR]

The Amhara region of Ethiopia is endowed with honey of diverse varieties and qualities. However, there is a lack of information on its secondary metabolite content and antioxidant nature. For this study, 47 fresh honey samples were collected from seven administrative zones throughout three provinces in the Amhara National Regional State, Ethiopia. The honey samples' restorative nature was evaluated by the quantitative determination of phenolic content and antioxidant capabilities using standard colorimetric methods. The finding showed that the mean values of total polyphenol content based on gallic acid equivalent (GAE) ranged from 17.03 to 42.04 mg GAE per 100 g of honey. The mean value of the entire flavonoid content using catechin equivalent (CE) was from 3.20 to 7.40 mg CE, and when using quercetin equivalent (QE), it ranged from 1.67 to 5.08 mg QE, per 100 g of honey sample. The ascorbic acid equivalent antioxidant content (AEAC) of the honey samples – ranged from 16.23 to 26.5 9 mg AEAC per 100 g of the honey samples. The percent antioxidant activities (% AA) of the honey samples—ranged from 23.74 to 40.11%. There was a strong positive correlation between phenolic content and antioxidant properties. Amber-colored honey enjoyed the highest value on the stated parameters based on the samples' colors, while the white-colored samples registered the least value. Based on the findings, it is concluded that the region's honey has a magnificent therapeutic nature. Using the principal component analysis (PCA) model, the top three principal components described 96.63% of the total variations. The linear discriminant analysis (LDA) model has an average of 68.1% discriminant power. The LDA model was cross-validated by the leave-one-out cross-validation approach, and 70.21% of it clustered adequately. In the biplot analysis, honey sample distribution based on their color clustered better than the geographic origin and climate factors. [ABSTRACT FROM AUTHOR]

Tejocote (Crataegus mexicana, Mexican hawthorn), known as a weight-loss supplement, has been marketed online and is easily available for overseas direct purchase. Alipotec (brand name) is known as one of the most popular products containing tejocote in Mexico and other countries. However, adverse effects have been reported by users of these supplements. Therefore it is necessary to find the reason for the side effect. Dietary supplement samples labelled as containing tejocote were analysed using mass spectrometry and DNA barcoding analysis. Our results demonstrate that Alipotec samples contained ingredients from different species, yellow oleander instead of tejocote. The rpoB barcode region was able to differentiate between tejocote and yellow oleander species. Moreover, it was also observed that three compounds, including thevetin B, neriifolin, and digitoxigenin, clearly distinguish between tejocote and yellow oleander samples. This is the first and preliminary investigation to use an integrated approach of both chemical and genomic profiling for the authentication of dietary supplement containing tejocote. [ABSTRACT FROM AUTHOR]

Contents of total flavonoids (TFc), total phenolics (TPc), and total crude polysaccharide (TCPc) in licorice from different origins were determined by optimized colorimetric methods, whereas five monomer ingredients (liquiritin [LQ], isoliquiritin [ILQ], liquiritigenin [LQG], isoliquiritigenin [ILQG], and glycyrrhizic acid [GA]) were simultaneously identified and quantified by HPLC–MS and HPLC. The results indicated that the contents of chemical compounds in licorice showed significant difference in different origins. Hierarchical cluster analysis and principal component analysis further proved that producing area indeed affected the quality including compounds and pharmacological activity in licorice. Licorice from Inner Mongolia exhibited the excellent DPPH assay, whereas samples from Gansu and Xinjiang showed high scavenging capacity to OH and ABTS free radicals. Meanwhile, α‐Glu inhibitory activity of licorice samples was four times higher than the antioxidant activity. Correlation analysis made clear that TFc and TCPc both strongly contribute to DPPH scavenge capacity at P < 0.01 level, whereas TCPc contributed to α‐Glu inhibitory activity at P < 0.05 level. This study would contribute to the comprehensive quality evaluation based on the compounds and pharmacological activity of licorice, and provide a reference for the choice of producing area to ensure the quality of licorice as a medicine. [ABSTRACT FROM AUTHOR]

Lichens are sources of numerous biologically active compounds and many of these have demonstrated antitumor potential. The purposes of this study were to evaluate the antiproliferative activity and selectivity of the following compounds isolated from lichens: atranorin and diffractaic, divaricatic, perlatolic, psoromic, norstictic, and protocetraric acids. Cytotoxicity tests based on sulforhodamine B were performed on normal cells (NIH/3T3, fibroblast) and cancer cell lines 786-0 (renal), MCF7 (breast), HT-29 (colon), PC-3 (prostate), and HEp2 (laryngeal). Diffractaic acid exhibited GI50 values in the 58.6-98.9 µM range. Divaricatic and perlatolic acids were the most active compounds, with GI50 values of 9.8 and 15.5 µM for PC-3 and MCF7 cells, respectively. Protocetraric acid proved active only against HEp2 cells (GI50 = 41.4 µM). Atranorin, psoromic acid, and norstictic acids were inactive against all the cells tested. Chemometrics was used to evaluate the effect of the compounds against the cell lines tested. PCA (Principal Component Analysis) based on GI50 values ​​separated compounds into two groups compared to doxorubucin, while HCA (Hierarchical Cluster Analysis) separated them into three groups based on SI values. DOI: http://dx.doi.org/10.17807/orbital.v12i1.1397

Due to problems with selenium deficiency in humans, the search for new organic molecules containing this element in plant biofortification process is highly required. Selenium organic esters evaluated in this study (E-NS-4, E-NS-17, E-NS-71, EDA-11, and EDA-117) are based mostly on benzoselenoate scaffolds, with some additional halogen atoms and various functional groups in the aliphatic side chain of different length, while one compound contains a phenylpiperazine moiety (WA-4b). In our previous study, the biofortification of kale sprouts with organoselenium compounds (at the concentrations of 15 mg/L in the culture fluid) strongly enhanced the synthesis of glucosinolates and isothiocyanates. Thus, the study aimed to discover the relationships between molecular characteristics of the organoselenium compounds used and the amount of sulfur phytochemicals in kale sprouts. The statistical partial least square model with eigenvalues equaled 3.98 and 1.03 for the first and second latent components, respectively, which explained 83.5% of variance in the predictive parameters, and 78.6% of response parameter variance was applied to reveal the existence of the correlation structure between molecular descriptors of selenium compounds as predictive parameters and biochemical features of studied sprouts as response parameters (correlation coefficients for parameters in PLS model in the range—0.521 ÷ 1.000). This study supported the conclusion that future biofortifiers composed of organic compounds should simultaneously contain nitryl groups, which may facilitate the production of plant-based sulfur compounds, as well as organoselenium moieties, which may influence the production of low molecular weight selenium metabolites. In the case of the new chemical compounds, environmental aspects should also be evaluated.

Olive tree crops and the olive oil market are becoming less and less diverse due to the rise of intensive growth varieties, with the consequent loss of varietal richness provided by oils from minority and autochthonous cultivars. “Royal de Calatayud” and “Negral de Sabiñán” are two local minority cultivars in Aragon (Spain). Fruit parameters such as ripening, fresh weight, and oil yield were evaluated, as well as physico-chemical and chemical composition parameters in olive oil in comparison with “Arbequina”, a cultivar widespread in Spain and other countries. Fruits were harvested from October to December in 2017 and 2019. Chemometric analysis revealed significant varietal differences among the three cultivars. In comparison with “Arbequina”, higher oil yields were obtained in the two local cultivars. “Royal de Calatayud” has a higher oleic acid content and a greater quantity of phenolic compounds. It thus displays a better nutritional profile than “Arbequina”. This preliminary study shows that “Royal de Calatayud” could be regarded as an excellent alternative to the “Arbequina” cultivar in the parameters analyzed.

Fritillariae cirrhosae bulbus (FCB) is one of the most important traditional Chinese medicines (TCM) for the treatment of cough and phlegm. Due to increasing demand and the complexity of FCB’s botanical origin, various substitutes have appeared in the market, resulting in a major challenge to distinguish FCB and its substitutes (F. pallidiflorae bulbus, FPB). Therefore, discriminating FCB from FPB has becoming an urgent necessity. In this study, an ultra-high-performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UPLC–ESI–MS/MS) method was developed for the simultaneous quantification of nine steroidal alkaloids (imperialine-3-β-D-glucoside, imperialine, verticine, verticinone, peimisine, yibeinoside A, delavine, delavinone, ebeidinone) within 8 min. According to the composition and content of the above nine compounds, multivariate chemometric analyses were applied for the classification of FCB and FPB. The quantitative results showed that there were both similarities and differences in the content of nine steroidal alkaloids between FCB and FPB, and it was difficult to directly distinguish these two species. Fortunately, with the aid of chemometric analyses, FCB and FPB were successfully differentiated by partial least squares discrimination analysis (PLS-DA) and orthogonal partial least squares discrimination analysis (OPLS-DA) models based on the nine alkaloids’ content. Moreover, four compounds (yibeinoside A, ebeiedinone, delavinone and imperialine) were discovered as potential markers for the identification and differentiation of FCB and FPB. Additionally, compared to other studies, this work collected a large number of samples (49 batches of FCB and 17 batches of FPB) to ensure the reliability of the results. In conclusion, this work established a new approach for the authentication of FCB based on its active components, which provides a good reference for the quality control of FCB and will help us to understand the chemical composition differences between FCB and its adulterants further.

Angelica dahurica is a famous functional food and herb. To guarantee quality of A. dahurica, a strategy “Q-markers targeted screening” was successfully developed by sufficient extraction of compounds and the targeted screening of qualitative and quantitative markers calculated through chemometric methods based fingerprints. Accelerated solvent extraction was selected due to its prominent advantages exhibiting the maximum extraction yields and varieties of compounds and especially excellent reproducibility (RSD