Spectroscopic Analysis Methods Research Articles

Fast spectroscopic and multisensor methods for analysis of glucosamine and hyaluronic acid in dietary supplements

Fast spectroscopic and multisensor methods for analysis of glucosamine and hyaluronic acid in dietary supplements

Unusual Composition of the Sarezzano Reliquary Busts

The interdisciplinary study of two reliquary busts from Sarezzano (Piedmont, Italy) is a perfect example of the necessity to provide for material characterisation as a recurring common practice in historical studies and a mandatory step in conservation assessment. Furthermore, the diagnostics of cultural heritage play a crucial role in art historical research, providing relevant information on artefacts’ genesis, production technology, and conservation history. The study of the materials of the reliquary busts was performed by non-invasive (portable X-ray fluorescence spectrometry) and micro-invasive (stereomicroscope, attenuated total reflection Fourier transform infrared spectroscopy and powder X-ray diffraction analysis) methods. According to the results, the busts were found to be made of a tin–lead alloy, a rather unusual material for mediaeval reliquary busts. Moreover, the outcome suggests that the busts were originally silvered, except for the hair and beard which are still gilded. The analysis reveals the use of colophony as an adhesive buffer layer on the busts’ alloy, as well as inside them, to favour the metal working process, since it is found as degraded residue. Finally, even the typology of alloy decay is defined. All this information has enabled us to determine the artistic technique and estimate the value and quality of the material employed. In addition, it has led to the correct choice of materials and methods to be adopted during the restoration, and therefore the usage of more suitable solvents and tools.

Studying of serum bile acids metabolomics as potential biomarkers for differentiation between hepatocellular carcinoma and cholangiocarcinoma

BackgroundMetabolomics is an emerging field that quantifies numerous metabolites systematically aiming to determine the metabolites corresponding to each biological phenotype and then provide an analysis of the mechanisms involved. Bile acids (as an organic metabolites) are synthesized in the liver from cholesterol and could be used as indicator of hepatobiliary impairment. However, the role of these bile acids in the pathogenesis of cholangiocarcinoma (CCA) and hepatocellular carcinoma (HCC) is still unclear. Therefore, the current study aimed to use serum bile acid profiles potential diagnostic biomarkers for early detection of cholangiocarcinoma and differentiating it from hepatocellular carcinoma.Subjects and methodsUltra-performance liquid chromatography-tandem mass spectrometry (UPLC/MS/ MS) analytical method was used for the measurement of bile acids in the serum of patients with hepatocellular carcinoma (n = 35), cholangiocarcinoma (n = 35), and control group (n = 35) to determine role as markers for differentiation between hepatocellular carcinoma and cholangiocarcinoma.ResultsThis study revealed that there was a significant increase in all 14 bile acids in both HCC and CCA compared to control. Also, there was significant increase in LCA, TCA, GDCA, and GCA in cholangiocarcinoma (CCA) compared to HCC with AUC 0.775, 0.825, 0.797, and 0.831 respectively with highest sensitivity and specificity for GCA (82% and 74%, respectively) for differentiation between the two types of cancers.ConclusionDetermination of the serum bile acids pattern using UPLC/MS/MS may help to differentiate between hepatocellular carcinoma (HCC) and cholangiocarcinoma (CCA) especially GCA which may be a good biomarker for differentiation between two types of liver cancers.

Evaluation of 1064 nm Raman for meat and bone meal species discrimination: From raw form to chemical and physical components

The 1064 nm Raman spectroscopy technique was employed to characterize raw, bone fragments (BF), meat fragments (MF), lipid, and residue of meat and bone meal (MBM) samples. Employing three chemometric algorithms, species discrimination models were optimized for the aforementioned sample types, indicating that the presence of BF favored discriminant analysis for poultry samples, yielding a classification error of 0.000. The species discrimination model constructed using Raman spectra combined with PLS-DA algorithm for residue samples was found to be overall optimal, with classification error for four species samples all below 0.061. A detailed analysis of the BF related spectral variables contributing significantly to PLS-DA discriminant analysis was conducted. Finally, this study established the complementarity of Raman spectroscopy in species discrimination analysis from both a physical and chemical components perspective, laying the theoretical groundwork for the development of a high-precision 1064 nm Raman spectroscopic analysis method for MBM species discrimination.

OBTAINING AN ACTIVE INGREDIENT FOR COTTON SEED TREATMENT BASED ON METHYLENDIUREA AND PARAAMINOBENZOIC ACID AND STUDYING ITS PHYSICOCHEMICAL CHARACTERISTICS

Seed treatment is the main method of protecting plants from infectious diseases. The article presents data on the production of a double compound based on methylene diurea and paraaminobenzoic acid and the study of its physicochemical characteristics. The chemical interaction in the three-component water-salt system methylenediurea (MDU) – para-aminobenzoic acid (PABA) – water was studied using the isothermal method of physicochemical analysis. The crystallization region of the new binary compound, the active substance, was established at a molar ratio MDU: PABA = 1:2. The formation of the double compound is confirmed by X-ray phase and IR spectroscopic methods of analysis. From the obtained X-ray phase analysis data, it follows that the reference lines of the double compound and their intensity differ from the X-ray patterns of the initial components. The IR spectra of MDM and PABA are characterized by intense absorption in the region of 3500-3390 cm-1 , 2000-500 cm-1 and 3500-3345 cm-1 , 1800-500 cm-1 , respectively. In the IR spectra of the new double compound MDM•2PABA, the absorption intensity in the region of 1800-500 cm-1 increases. A decrease in the absorption region of the stretching vibration of CO groups from 1626, 1626.3 cm-1 to 1612 cm-1 is observed in the case of the double compound MDM•2PABA. The results of the studies indicate the formation of a new compound. It is shown that the double compound has low hygroscopicity under summer, autumn, spring and winter storage conditions, high swelling and moisture capacity, and low solubility.

Catalytic Ozonation Treatment of Coal Chemical Reverse Osmosis Concentrate: Water Quality Analysis, Parameter Optimization, and Catalyst Deactivation Investigation.

Catalytic ozone oxidation, which is characterized by strong oxidizing properties and environmental friendliness, has been widely used in organic wastewater treatments. However, problems such as a low organic pollutant removal efficiency and unstable operation during the catalytic ozone treatment process for wastewater remain. To address these disadvantages, in this study, the treatment efficacy of catalytic ozone oxidation on a coal chemical reverse osmosis concentrate was investigated. The basic water quality indicators of the chemical reverse osmosis concentrate were analyzed. The effects of initial pollutant concentration, pH, ozone concentration, and catalyst concentration on the COD removal rate from the coal chemical reverse osmosis concentrate were explored. Water quality indicators of the chemical reverse osmosis concentrate before and after the catalytic ozone treatment were studied using spectroscopic analysis methods. The RO concentrate demonstrated large water quality fluctuations, and the catalytic ozonation process removed most of the pollutants from the treated wastewater. A possible deactivation mechanism of the ozone catalyst was also proposed. This study provides a theoretical reference and technical support for the long-term, efficient, and stable removal of organic pollutants from coal chemical reverse osmosis concentrate using a catalytic ozone oxidation process in practical engineering applications.

Terpenoids and steroids from aerial parts of Achillea alpina L. as PTP1B inhibitors: Kinetic analysis and molecular docking studies

Achillea alpina L. (Alpine yarrow) is a noteworthy herb in the genus Achillea with many uses in vegetables and traditionally used to treat stomach disorders. In our continuous research on the chemical constituents and biological activities of medicinal plants, ten previously undescribed terpenoids including eight eudesmane-type sesquiterpenes (1–8), one nor-eudesmane-type sesquiterpene (9), one cyclo-geraniol derivative (10), and twenty-one known compounds were isolated and structurally elucidated from the aerial parts of A. alpina. Structures and absolute configurations of the undescribed terpenoids were identified using comprehensive spectroscopic analysis (NMR, HRESI-MS, and CD data) and computational methods (ECD and NMR calculation). Enzyme inhibitory assays showed that the isolated sesquiterpene (19), triterpene (22), and sterol (26) were protein tyrosine phosphatase 1B (PTP1B) inhibitors with IC50 values ranging from 14.87 to 23.09 μM in comparison with positive control - ursolic acid, showing IC50 value of 5.93 ± 0.16 μM. Further enzyme kinetics and molecular docking studies were performed to provide valuable insights into their mechanism of action.

SOLUBILITY POLYTEREME OF THE SYSTEM AMMONIUM SULPHATE - MAGNESIUM CHLORATE DEFOLIANT - WATER

The mutual influence of components in an aqueous system consisting of ammonium sulfate and magnesium chlorate defoliant was studied in a wide concentration range at a temperature of -27.0 to 4.5°C. On the state diagram of the system, the fields of crystallization of ice, magnesium chlorate hexahydrate, ammonium sulfate, and the compound (NH4)2SO4 ∙ 2NH4CIO3 ∙ 2MgSO4 ∙ H2O are delimited, which was identified and characterized by chemical, X-ray phase, thermal, and IR spectroscopic methods of analysis.

Investigation of the Process of Agglomeration of Phosphorites Using Phosphate-Siliceous Shales and Oil Sludge

Introduction This article aims to discuss the physico-chemical features of the agglomeration process of phosphorus fines using phosphate-siliceous shales and oil sludge. Methods The composition and structure of the starting materials and physico-chemical transformations under thermal influence are studied using IR spectrometry and differential thermal analysis methods. Results The results of IR spectrometric analysis of the phosphate siliceous shales are characterized by intense peaks at 493.78, 547.78, and 678.94 cm-1, corresponding to Ca-O-P compounds. Moreover, the wave oscillations in the region of 837.11-995.27 cm-1 indicate the characteristics of Si-O valence bonds, and in the region of 1114.86-1431 cm-1 depict the characteristics of Si-O-Al compounds. The IR spectrum of oil sludge is characterized by the presence of wave oscillations in the region of 1411.89-2904.80 cm-1 corresponding to petroleum components. Conclusion The differential thermal analysis of the investigated sample of phosphate-siliceous shale does not have intense endo- and exo-effects, and it is characterized by a significant predominance of hydrate compounds of aluminosilicate and carbonate components.

Heavy metal levels of outdoor dust from the Eastern Mediterranean Sea region and assessment of the ecological and health risk.

As a result of some chemical element (heavy metals) pollution of dust, environmental pollution of dust has become an increasing concern, necessitating an assessment of risks to both ecology and human health, particularly in urban areas. Most of these pollutants settle on the outdoors and eventually become part of the outdoor dust. These will have negative long-term repercussions on ecosystems and human health. In this research, energy dispersive X-ray fluorescence (EDXRF) spectrometry analytical method was used to assess the pollution characteristics of the eight heavy metals (HMs): Mn, Cu, As, Hg, Ni, Cr, Zn, and Pb in the East Mediterranean Sea area. The concentration of As, Mn, Cr, Cu, Hg, Ni, Pb, and Zn analyzed in outdoor dust samples varied from 0.94 to 19.52 mg kg-1, 190.08 to 1019.7 mg kg-1, 20.46 to 45.9 mg kg-1, 19.5 to 62.56 mg kg-1, 0.01 to 0.93 mg kg-1, 10.48 to 40.64 mg kg-1, 12. 6 to 36.1 mg kg-1, and 48.96 to 112.41mg kg-1, respectively. HMs have been detected in the outdoor dust samples analyzed in the study, and, as a result, mean concentrations followed the order Mn > Zn > Cu > Cr > Ni > Pb > As > Hg, respectively. The ecological risk was observed at various contamination levels, with As and Hg pollution being the most severe. The highest hazard quotient (HQ) for adults and children was determined as a result of As and Cr, respectively. According to the US-EPA health risk threshold, the cancer risk in the study area is negligible.

A spectroscopic analysis code for spatially resolved x-ray absorption data from the COAX platform.

Sophisticated tools such as computer vision techniques in combination with 1D lineout type analyses have been used in automating the analysis of spectral data for high energy density (HED) plasmas. Standardized automation can solve the problems posed by the complexity of HED spectra and the quantity of data. We present a spectroscopic code written for automated and streamlined analysis of spatially resolved x-ray absorption data from the COAX platform on Omega-60. COAX uses radiographs and spectroscopic diagnostics to provide shock position and density information. We also obtain the more novel spectral-derived spatial profile of the supersonic radiation flow into a low-density foam. Considerable effort has been spent modernizing our previous spectroscopic analysis method, including the development of new tools characterized by a faster runtime and minimal user input to reduce bias and a testing suite for verifying the accuracy of the various functions within the code. The new code analyzes our spectroscopic images in 1-2min, with added uncertainty and confidence.

Identification of Alzheimer’s disease and vascular dementia based on a Deep Forest and near-infrared spectroscopy analysis method

Alzheimer’s disease (AD) and vascular dementia (VaD) typically do not exhibit distinct differences in clinical manifestations and auxiliary examination results, which leads to a high misdiagnosis rate. However, significant differences in treatment approaches and prognosis between these two diseases underscore the critical need for an accurate diagnosis of AD and VaD. In this study, serum samples from 33 patients with AD patients, 37 patients with VaD, and 130 healthy individuals were collected, employing near-infrared aquaphotomics technology in combination with deep learning for differential diagnoses. Through an analysis of water absorption patterns among different diseases via aquaphotomics, the efficacies of traditional machine learning methods (Support Vector Machine and Decision Trees) and deep learning approaches (Deep Forest) in modeling were compared. Ultimately, by leveraging feature extraction techniques in conjunction with deep learning, a differential diagnostic model for AD and VaD was successfully developed. The results revealed that aquaphotomics could identify a certain correlation between the number of hydrogen bonds in water molecules and the development of AD and VaD; the deep learning model was found to be superior to traditional machine learning models, achieving an accuracy of 98.67 %, sensitivity of 97.33 %, and specificity of 100.00 %. The bands identified using the Competitive Adaptive Reweighting Algorithm method, primarily located at approximately 1300–1500 nm, showed a significant correlation with water molecules containing four hydrogen bonds. These results highlighted the potential role of the water molecule hydrogen-bond network in disease development and were consistent with the aquaphotomics analysis results. Therefore, the differential diagnostic model developed by integrating near-infrared spectroscopy and deep learning was proven to be effective and feasible, providing accurate and rapid diagnostic methods for AD and VaD diagnoses.

Diterpenoids with Potent Anti-Psoriasis Activity from Euphorbia helioscopia L.

Psoriasis, an immune-mediated inflammatory skin disorder, seriously affects the quality of life of nearly four percent of the world population. Euphorbia helioscopia L. is the monarch constituent of Chinese ZeQi powder preparation for psoriasis, so it is necessary to illustrate its active ingredients. Thus, twenty-three diterpenoids, including seven new ones, were isolated from the whole herb of E. helioscopia L. Compounds 1 and 2, each featuring a 2,3-dicarboxylic functionality, are the first examples in the ent-2,3-sceo-atisane or the ent-2,3-sceo-abietane family. Extensive spectroscopic analysis (1D, 2D NMR, and HRMS data) and computational methods were used to confirm their structures and absolute configurations. According to the previous study and NMR data from the jatropha diterpenes obtained in this study, some efficient 1H NMR spectroscopic rules for assigning the relative configurations of 3α-benzyloxy-jatroph-11E-ene and 7,8-seco-3α-benzyloxy-jatropha-11E-ene were summarized. Moreover, the hyperproliferation of T cells and keratinocytes is considered a key pathophysiology of psoriasis. Anti-proliferative activities against induced T/B lymphocytes and HaCaT cells were tested, and IC50 values of some compounds ranged from 6.7 to 31.5 μM. Compounds 7 and 11 reduced the secretions of IFN-γ and IL-2 significantly. Further immunofluorescence experiments and a docking study with NF-κB P65 showed that compound 13 interfered with the proliferation of HaCaT cells by inhibiting the NF-κB P65 phosphorylation at the protein level.

Recent Research Progress on the Chemical Constituents, Pharmacology, and Pharmacokinetics of Alpinae oxyphyllae Fructus.

Alpinae oxyphyllae fructus (AOF), the dried mature fruit of Alpinia oxyphylla Miquel of the Zingiberaceae family, shows many special pharmacological effects. In recent years, there has been an abundance of research results on AOF. In this paper, the new compounds isolated from AOF since 2018 are reviewed, including terpenes, flavonoids, diarylheptanoids, phenolic acid, sterols, alkanes, fats, etc. The isolation methods that were applied include the microwave-assisted method, response surface method, chiral high-performance liquid chromatography-multiple reaction monitoring-mass spectrometry (HPLC-MRM-MS) analytical method, ultra-high-performance liquid chromatography-quadrupole-electrostatic field orbitrap high-resolution mass spectrometry (UPLC-Orbitrap-HRMS) method, ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method, hot water leaching method, ethanol leaching method, and so on. Additionally, the pharmacological effects of AOF found from 2018 to 2024 are also summarized, including neuroprotection, regulation of metabolic disorders, antioxidant activity, antiapoptosis, antiinflammatory activity, antidiabetic activity, antihyperuricemia, antiaging, antidiuresis, immune regulation, anti-tumor activity, renal protection, hepatoprotection, and anti-asthma. This paper provides a reference for further research on AOF.

ESTIMATION OF TENOFOVIR BY UV VISIBLE SPECTROSCOPY

In view of the need for a suitable Spectroscopic method for routine analysis of Tenofovir(antiretroviral medicine) in formulations, attempts were made to develop simple, precise and accurate analytical method for estimation of Tenofovir in formulation. As Validation is a necessary and important step in both framing and documenting the capabilities of the developed method it was done in accordance with USP and ICH guideline for the assay of active ingredient. The method was validated for parameters like linearity, precision, accuracy, specificity, and robustness, limit of detection and limit of quantification. This method provides means to quantify the component. This proposed method was suitable for the analysis of Pharmaceutical dosage forms.The utility of the developed method to determine the content of drug in commercial formulation was also demonstrated. KEY WORDS: Tinofovir,Validation,UV Visible spectroscopy.

Determination of Choline-Containing Compounds in Rice Bran Fermented with Aspergillus oryzae Using Liquid Chromatography/Tandem Mass Spectrometry.

Choline-containing compounds are essential nutrients for human activity, as they are involved in many biological processes, including cell membrane organization, methyl group donation, neurotransmission, signal transduction, lipid transport, and metabolism. These compounds are normally obtained from food. Fermented brown rice and rice bran with Aspergillus oryzae (FBRA) is a fermented food product derived from rice and rice ingredients. FBRA exhibits a multitude of functional properties with respect to the health sciences. This study has a particular focus on choline-containing compounds. We first developed a simultaneous liquid chromatography/tandem mass spectrometry (LC/MS/MS) analysis method for seven choline-containing compounds. The method was subsequently applied to FBRA and its ingredients. Hydrophilic interaction chromatography (HILIC) and selected reaction monitoring were employed for the simultaneous analysis of seven choline-containing compounds. MS ion source conditions were optimized in positive ion mode, and the product ions derived from the choline group were obtained through MS/MS optimization. Under optimized HILIC conditions, the peaks exhibited good shape without peak tailing. Calibration curves demonstrated high linearity across a 300- to 10,000-fold concentration range. The application of the method to FBRA and other ingredients revealed significant differences between food with and without fermentation. In particular, betaine and α-glycerophosphocholine were found to be highest in FBRA and brown rice malt, respectively. The results indicated that the fermentation processing of rice ingredients results in alterations to the choline-containing compounds present in foods. The developed HILIC/MS/MS method proved to be a valuable tool for elucidating the composition of choline-containing compounds in foods.

Prenyl Pterocarpans from Algerian Bituminaria bituminosa and Their Effects on Neuroblastoma.

The pterocarpan fraction from aerial parts of Bituminaria bituminosa was investigated for both chemical characterization and biological evaluation. Chemical studies were in accordance with the literature data on Bituminaria genus resulting in the identification of typical 4,8-prenyl pterocarpans. Three new members, bituminarins A-C (1-3), were isolated along with main bitucarpin A (4), erybraedin C (5) and erybraedin D (6) already reported from this plant. Further, biological studies evidenced antiproliferative properties of the most abundant pterocarpans 4 and 5 on neuroblastoma SH-SY5Y cell line, in agreement with previously described antiproliferative activity of these compounds against cancer cell lines other than neuroblastoma. The structure and the stereochemistry of the new molecules was determined by extensive spectroscopic analysis and chemical derivatization methods. The biological investigation was carried out by using an assay platform based on a live-cell imaging system revealing an apoptotic cell death induction.

Four new phenylpropanoid glycosides from the leaves of Illicium dunnianum and their neuroprotective activities

Four previously unreported phenylpropanoid glycosides (1–4), together with four known analogues (5–8), were isolated from the leaves of Illicium dunnianum. The structures of these new compounds were elucidated based on spectroscopic analysis (HR-ESI-MS, NMR, IR, UV) and chemical methods. In addition, the neuroprotective activities of all the isolates were evaluated by measuring their cell viability in H2O2-induced OLN-93 cell injury model.

Label-free surface-enhanced Raman spectroscopy analysis method for liquid biopsy and its application in serum-based lung cancer diagnosis and classification

Liquid biopsy offers promise for the diagnosis of malignant tumors or their precancerous lesions at the subclinical stage, which is crucial for improving the survival rate of cancer. Label-free surface-enhanced Raman spectroscopy (SERS) has become an emerging detection method in liquid biopsy. The accuracy of SERS-based diagnosis relies on both precise measurement and effective data analysis. In our previous study, a large laser spot SERS method was proposed for the precise detection of complex liquids. In this work, a logical Raman data analysis method was developed, to address the lack of Raman characteristics and biological significance in current SERS-based diagnosis data analysis. The measured Raman data is classified to obtain a weighting matrix of classification criteria, and this matrix is used to establish a material correspondence with the Raman spectra, extract key Raman peaks, determine corresponding biomolecules and biological processes, thus enabling a logical analysis of the data. This method has been used to analyze the SERS data of lung cancer, it can not only show exceptional performance in diagnosing lung cancer and differentiating small cell lung cancer, but also obtain the Raman diagnostic and classification criteria with clear numerical values and reasonable biological significance, demonstrating its great potential value in precise biosensing.

One new triterpene glycoside from Cyclocarya paliurus

One previously undescribed triterpene glycoside (1) and two known compounds were isolated from the leaves of Cyclocarya paliurus (2-3). Their structures were elucidated based on methods of spectroscopic analysis and NMR data comparison with those in the literature. Compound 1 showed a moderate inhibitory effect on melanogenesis with an IC50 value of 282.3 μM, with the positive drug arbutin showing an IC50 value of 168.5 μM.