Semiquantitative Determination Research Articles

Analysis of the subcapital two-part humerus fracture by fluoroscopy: objective criteria for classification and decision making

BackgroundSurgical decision making in the treatment of proximal humerus fractures (PHFx) is primarily based on fracture classification using standard radiographs. Due to the lack of objective criteria, this classification process is associated with high interobserver variation. In this study, we investigate the fluoroscopic analysis of humerus fractures through the surgical neck using a semi-quantitative determination of distinct angulation patterns of the proximal humerus as they appear in the image intensifier.MethodsUsing a saw bone model, defined subcapital 2-part fracture configurations were generated and assessed radiographically. Anatomical landmarks—including the greater and lesser tuberosity as well as anatomical neck—were identified using an image converter, and the exact degree of fracture displacement with 10° up to 70° (in 10° increments) of posterior, varus or combined posterior-varus angulation was compared to nondisplaced controls. From the resultant series of radiographs, the appearance of these angulations in anteroposterior (AP) and scapular Y-views were also visualized and defined.ResultsAn angulation of 50° or more of any given 2-part fracture through the surgical neck is present when the greater tuberosity becomes the most proximal point in AP view (varus and combined posterior-varus angulation) or a bimodal form is found for the superior contour of the head with the lesser tuberosity being the most proximal point in the Y-view (posterior angulation).ConclusionThe radiological appearance of various PHFx constellations can be well visualized using the saw bone shoulder model. The presence of angulation in accordance with the Neer classification for group III fractures can be adequately determined by analyzing the relative position of the greater or lesser tuberosity to the humeral head calotte. This can assist the surgeon’s decision on whether to operate or opt for a conservative approach.Level of evidenceBasic Science, Anatomy Study, Imaging.

Laboratory signs of carbohydrate malabsorption in early age children with rotavirus infection

The aim – to determine the laboratory manifestations of carbohydrate malabsorption syndrome in the dynamics of rotavirus infection in early age children and to identify the factors that influence its severity. Materials and methods. The study included 60 breastfed children aged 1–24 months with rotavirus infection, who underwent pH-metry of feces, semi-quantitative determination of total carbohydrates (Benedict’s method), lactose (Malfatti method) and glucose (test systems Glucophan) in feces on the 2nd, 3rd, 5th, 7th and 10th days of the disease. Results. Carbohydrate malabsorption syndrome was observed in 98.3% of patients. The level of fecal carbohydrates increased on the second-third day to a clinically significant 0.50 [0.20; 1,50] %, reached its maximum in the midst of the disease – from the fifth to the seventh day (0.75 [0.50; 1.65] % and 0.87 [0.40; 1.65] %, respectively), decreasing during convalescence to 0.50 [0.20; 1.50] % (P < 0.05 relative to the 10th day), but remained elevated in 81.7 % of patients (P < 0.05 relative to healthy children). Lactase deficiency and glucose malabsorption (P < 0.05 relative to healthy children) were observed throughout the RVI period. At all stages of RVI there was a strong direct correlation between the total level of carbohydrates and lactose in the feces (on the second, third, fifth, seventh and tenth days r = 0.91; r = 0.86; r = 0.91; r = 0.89, respectively). The age dependence of the severity of laboratory indicators of carbohydrate malabsorption was established. Children in the first 6 months had the highest maximum levels of carbohydrates and fecal lactose – 1.75 [1.00; 2.00] % and 3.50 [2.00; 4.00] + respectively (P < 0.05 relative to 12–24 months children) and significantly higher values of these indicators in the dynamics of RVI (P < 0.05 relative to 12–24 months children) for the second-third, fifth and the tenth day). Children with concomitant food allergies, atopic dermatitis and iron deficiency anemia had 2.0 and 1.5 times higher maximum levels of carbohydrates and lactose in the stool, respectively (P < 0.05), as well as higher values of these indicators in the dynamics of the disease – on the third and fifth days (P < 0.05). Conclusions. The vast majority of young patients with rotavirus infection have carbohydrate malabsorption syndrome, which occurs from the first days of the disease and is most pronounced on the fifth to seventh day (P < 0.05 relative to the 10th day), realized mainly due to lactase deficiency. The most pronounced carbohydrate malabsorption syndrome and lactase deficiency in the dynamics of the disease are present in children of the first six months of life. Factors that increase the severity of carbohydrate malabsorption due to secondary lactase deficiency in the acute period of rotavirus infection are concomitant food allergies, atopic dermatitis and iron deficiency anemia.

Hyperspectral sensor: A handy tool to evaluate the efficacy of cleaning procedures

• ASD-FieldSpec® 3 operates VNIR and SWIR reflectance spectral range. • VNIR and SWIR provide ready-to-use information on the degree of sulphation of carbonate stone. • SWIR data allowed information on efficacy of three different cleaning techniques. • The method supports monitoring of stone alteration during restoration. In urban environments, degradation processes affecting both natural and artificial carbonate materials commonly result in the formation of sulphate-based deposits (i.e., black crusts). Hyperspectral techniques may provide ready-to-use information on the degree of sulphation of carbonate stone, hence helping to monitor the conservation state of carbonate stone monuments. In this study, the Short-Wave InfraRed (SWIR) hyperspectral technique was tested on the world-famous marble-made Loggia di Baccio d’Agnolo in Santa Maria del Fiore Cathedral of Florence (Italy), affected by extensive “black crust” formation. A SWIR method based on a portable spectroradiometer (ASD Fieldspec® 3) was applied to verify the efficacy of different cleaning methods (i.e., laser, chemical and microbial). The interpretation of the SWIR spectra was based on a full-profile approach, in which the calcite and gypsum contributions were evaluated by weighing the best fit simulated contributions of reference compounds. The technique was able to provide in real time semi-quantitative determinations of the amount of gypsum developed on the stone surface, demonstrating to be a fast and handy routine tool during restoration of artworks.

Test methods for determining cationic and anionic surfactants in disinfecting and technological solutions

The purpose of the work was to develop Express methods for determining cationic and anionic surfactants in disinfectants and process solutions. The surfactant concentration was determined visually and colorimetrically by the intensity of color of the indicator zones of paper test strips or by the length of the colored (discolored) zones of test strips laminated in a polymer film. Semi-quantitative determination of surfactants in solutions was carried out by the intensity of color of the zones of indicator test strips pasted on the substrate (test titration on paper). Bromphenol blue was used as an indicator. The titrant was sodium dodecyl sulfate for cationic surfactants and cetylpyridinium chloride for anionic surfactants. Test strips were used for the determination of surfactants in the disinfectant solutions. The concentration in the range of 0.1 – 1.2% was determined by comparing the color with the standard color scale. The duration of the analysis was 3 – 5 min. Quantitative determination of surfactants was carried out by the length of the colored (discolored) zones of test strips glued in a polymer film. As an indicator for cationic surfactants, bromphenol blue (blue zone on the test strip) was used, and for anionic surfactants, an associate of bromphenol blue with cetylpyridinium chloride (discolored zone on the test strip). The determination range of the surfactant made up 16 – 1000 mg/liter. The concentration was determined according to a calibration graph representing the dependence of the length of the blue/discolored zone of the test strips on the concentration of surfactants in the solution. The relative standard deviation of the analysis results does not exceed 0.3; the analysis duration was 20 – 30 min.

Influence of the fatty acid profile on the volatile components of virgin olive oil subjected to thermal stress.

Virgin olive oil (VOO) is greatly appreciated for its organoleptic features, which can be ascribed mainly to the presence of very chemically diverse volatile components. It is well known that the VOO volatile fraction depends strongly on different aspects, which encompass genetic, agronomic, processing, and post-processing factors. In this research, we developed a method for the qualitative and semiquantitative determination of volatile components in VOOs subjected to thermal stress by headspace extraction online coupled to gas chromatography-mass spectrometry (HS-GC-MS). The method was applied to 100 extra-virgin olive oil (EVOO) samples, which led to the tentative identification of 52 volatile components, including 12 alcohols, 17 aldehydes, three ketones, one ether, two furans, two carboxylic acids, and 15 hydrocarbons. The method was used to study the cultivar effect and the main biochemical pathways involved in the synthesis of volatile compounds, with special emphasis on those formed by degradation of unsaturated fatty acids (FAs). Principal component analysis (PCA), explaining 76.7% of the total variability, showed that the volatile profile of EVOOs subjected to thermal stress allowed discriminating samples from different cultivars. Volatiles detected in EVOOs subjected to thermal stress with the highest contribution to discrimination between the selected cultivars were correlated with the concentration of the three main FAs in VOO, namely oleic, linoleic, and linolenic acids. The FA profile seems to be especially relevant to explain the concentration of certain volatile compounds with direct incidence on the organoleptic properties. © 2021 Society of Chemical Industry.

Effect of amines on formation of gold/polyurethane foam nanocomposites and its sensing opportunities

Effect of amines on formation of gold nanoparticles (AuNPs)/polymer nanocomposites has been observed and studied. Nanocomposites based on polyurethane foam and AuNPs were synthesized by interaction between the polymer modified with sodium borohydride and aqueous solution of tetrachloroauric acid. It has been shown that some amines cause a remarkable decrease of the surface plasmon resonance band of AuNPs in the nanocomposite material. Both aliphatic and aromatic amines as well as amines containing several amino groups were studied. A possible mechanism of the effect is discussed. It is probably based on stabilization of AuNPs with an amine that entails a decrease in the degree of their adsorption on PUF and appearance of the stabilized AuNPs in solution. The decrease of the nanocomposite surface plasmon resonance band is proportional to the concentration of amine in the solution. Based on this effect, a method for the determination of cetylamine, β-naphthylamine and neomycin in water and medical formulations using a monitor calibrator as a portable household tool is proposed. Under the selected conditions, the detection limits for amines were in the range of 0.7–1.5 μM, the determination ranges were approximately an order of magnitude. The observed color change of the nanocomposite samples also provides a good basis for semiquantitative determinations.

Bioanalysis of erlotinib, its O-demethylated metabolites OSI-413 and OSI-420, and other metabolites by liquid chromatography-tandem mass spectrometry with additional ion mobility identification

Erlotinib is a first-generation epithelial growth factor receptor inhibitor used in the treatment of non-small cellular lung cancers. Our previously published method on a Thermo TSQ Quantum Ultra triple quadrupole mass spectrometer for the quantitation of erlotinib, OSI-420, and OSI-413 and some other kinase inhibitors was transferred to a more sensitive Sciex QTRAP5500 system. Both methods showed comparable performance in the previous range (5–5000 and 1–1000 ng/mL for erlotinib and OSI-420) with comparable accuracies and precisions (98.9–106.2 vs 98.7.0–104.0, and 3.7–13.4 vs 4.6–13.2), and a high level of agreement between the methods (R2 = 0.9984 and 0.9951) for the quality control samples. The new system however was also capable of quantifying lower concentrations of both erlotinib and OSI-420 (0.5 and 0.1 ng/mL) with sufficient accuracy and precision. Along with the increased sensitivity we included the semi-quantitative determination of additional erlotinib metabolites M2, M3, M5, M6, M7, M8, M9, M10, M11, M12, M16 (hydroxy-erlotinib), M17, M18, M19, M20, M21 in a 0.1–1000 ng/mL range to the method. With a simple crash, dilute, and shoot sample preparation with acetonitrile and a 4.5 min analytical run time the method outperformed most other published methods in speed and simplicity and was suitable for TDM. Further, enhancement of the understanding of the pharmacokinetics of erlotinib and its metabolites was demonstrated.

Scanning densitometry and mass spectrometry for HPTLC analysis of lipids: The last 10 years

This work is a review on HPTLC contribution to lipid analysis in complex matrices, in the period from 2010 to now, lapse of time where hyphenation with other techniques, especially Mass Spectrometry, has experienced an important growth. Scanning densitometry (SD)-UV/FL of separated lipids, as the core of detection and centerpiece for hyphenation, and its coupling with MS using soft ionization techniques (ESI, APCI, MALDI, DESI and others), are the central axis of this work. The occasional intercalation in this coupling of an on-plate biological assay for effect-direct analysis (EDA) of lipids, as well as the combination of SD with radio-densitometry (RD) using isotopically labeled-lipids are also covered topics. The described techniques make possible to develop strategies for obtaining qualitative and different levels of quantitative information, including untargeted lipids species. HPTLC of lipids has been used for: comparative purposes; fingerprinting; semi-quantitative determination, identification of species; or quantitative determination of a given individual lipid. Goals in molecular biology and biochemistry-related samples have been: preparative isolations; control of purity; verification of metabolic products; on-plate biological assays; profiles in cells; analysis of products from the cellular metabolism; measurement of enzymatic activities; monitoring lipid transport across membranes or at biological interfaces; or monitoring lipid dynamics. Abbreviations: AcH: acetic acid; AMD: Automated Multiple Development; APCI: Atmospheric Pressure Chemical Ionization; Cer: Ceramides; Chol: Cholesterol; CholE: Cholesteryl esters: CholS: Cholesteryl sulfate; DCM: Dichloromethane; DESI: Desorption Electrospray Ionization; DG: Diacylglycerides; E1: estrone; E2: 17-β estradiol; E3: estriol; EE2: 17-α ethynylestradiol; EDA: Effect-Direct Analysis; ESI: Electrospray Ionization; EtOH: ethanol; FA: Fatty Acids; FAME: Fatty acid-methyl esters; FFA: Free Fatty Acids; GalCer: Galactosyl-Ceramides; Gb3: Globotriaosylceramides; Gb4: Globotetraosylceramides; GC: Gas Chromatography; GL: Glyco-lipids; GlcCer: Glucosyl-Ceramides; GSL: Glycosphingolipids; HPTLC: High-Performance Thin-Layer Chromatography; IMS: Ion-Mobility Separation; LacCer: Lactosyl-Ceramides; LC: Liquid Chromatography; LESA: Liquid Extraction Surface Analysis; LPC: Lyso-Phosphatidylcholines; LPG: Lyso-Phosphatidylglycerols; MALDI: Matrix Assisted Laser Desorption Ionization; m.d.: Migration distance; MeOH: Methanol; MG: Monoacylglycerides; NL: Neutral Lipids; PA: Phosphatidic Acids; PC: Phosphatidylcholines; PE: Phosphatidylethanolamines; PG: Phosphatidylglycerols; PI: Phosphatidylinositols; PL: Glycerophospholipids; PMA: Phosphomolybdic acid; PS: Phosphatidylserines; SD: Scanning Densitometry; SL: Sphingolipids; SM: Sphingomyelins; SQ: Semi-quantitative; Sq: squalene; SterylE: Steryl-esters; TG: Triacylglycerides

Active GTPase Pulldown Protocol.

Ras and its related small GTPases are important signalling nodes that regulate a wide variety of cellular functions. The active form of these proteins exists in a transient GTP bound state that mediates downstream signalling events. The dysregulation of these GTPases has been associated with the progression of multiple diseases, most prominently cancer and developmental syndromes known as Rasopathies. Determining the activation state of Ras and its relatives has hence been of paramount importance for the investigation of the biochemical functions of small GTPases in the cellular signal transduction network. This chapter describes the most broadly employed approach for the rapid, label-free qualitative and semi-quantitative determination of the Ras GTPase activation state, which can readily be adapted to the analysis of other related GTPases. The method relies on the affinity-based isolation of the active GTP-bound fraction of Ras in cellular extracts, followed by its visualization via western blotting. Specifically, we describe the production of the recombinant affinity probes or baits that bind to the respective active GTPases and the pulldown method for isolating the active GTPase fraction from adherent or non-adherent cells. This method allows for the reproducible measurement of active Ras or Ras family GTPases in a wide variety of cellular contexts.

Elevated Creatinine Clearance in Lupus Nephritis patients with Normal Creatinine.

Objectives: The present study aimed to observe the differences in creatinine clearance (Ccr) in systemic lupus erythematosus (SLE) patients with normal serum creatinine at different levels of urinary protein.Method: The present cross-sectional study included 177 SLE patients with normal serum creatinine from Qilu Hospital of Shandong University between January 2010 and April 2020. The following data were collected: blood urea nitrogen (BUN), serum creatinine (Cr), serum total protein, serum albumin, immunoglobulin (Ig) G, IgA, IgM, complement 3, complement 4, anti-ds-DNA antibody, routine urine test, urine protein/creatinine ratio (UPCR) (g/g), and the SLE disease activity index. The estimated Ccr was calculated according to the Cockcroft formula.Results: 123 patients were with positive urinary protein (Lupus Nephritis, LN group) and 54 patients were with negative urinary protein (Non-LN group). Compared with the Non-LN group, the LN group had higher BUN (5.76±3.22 vs. 4.78±1.58, P=0.007) and Cr (62.36±19.53 vs. 54.83±11.09, P=0.001). There was a strong correlation between the UPCR and the semi-quantitative determination of urine protein in LN patients (r=0.9583, P=0.0417). The serum creatinine levels were significantly higher in patients with urine protein 3+ (72.97±25.16) or massive proteinuria (62.32±19.66) than the other groups. Patients with urinary protein ± exhibited a significantly elevated Ccr when compared to patients with urinary protein 3+ (130.6±44.15 vs. 110.5±33.50, P=0.02), and patients with UPCR<0.15 g/g had higher Ccr than other groups and showed significantly increased Ccr compared with patients with UPCR≥0.15 g/g (132.44±21.02 vs. 115.14±35.89, P=0.007).Conclusions: Early renal function impairment may be present in LN patients. The kidneys of LN patients with urinary protein ± or UPCR<0.15 g/g are in a state of hyperfunction.

A fluorescence color card for point-of-care testing (POCT) and its application in simultaneous detection.

Diabetes mellitus has received much attention because its complications include liver, kidney, eye, heart and cerebrovascular diseases. Thus, it would be highly significant to develop a rapid and efficient method for glucose detection in biological samples. In this work, a point-of-care testing (POCT) method of glucose detection was proposed using a standard colorimetric card for semi-quantitative determination patterns. In the prepared fluorescence color card for glucose, a good linear relationship was acquired by plotting the ratio of the grayscale value (I/I0) versus the logarithm of glucose concentration within 100.0 to 1000.0 μmol L-1, and the LOD of glucose detection was 1.1 μmol L-1. A large number of actual samples (30 serum and 7 urine) were analyzed and the results demonstrated that this method had good potential to be applied in the primary screening of diabetic patients. In addition, this method is universal and can be applied in the simultaneous detection of multiple small molecules. It provides a new strategy for the primary screening of multiple diseases simultaneously, which presents excellent application potential.

Commercially available color-catching sheets for magnetic textile solid phase extraction of water-soluble dyes

Magnetic textile solid phase extraction, based on the use of magnetically separable color-catching sheets, was successfully employed for the preconcentration of water-soluble dyes methylene blue and crystal violet from water solutions. The photos of color-catching sheet squares with the adsorbed dye were taken with a mobile phone. The computer-based image analysis of the photos was performed using ImageJ freeware while smartphone-based image analysis employed On Color Measure application. The values of saturation from HSB (hue – saturation – brightness) color space, as well as red channel values from RGB (red – green – blue) color space were proportional to the methylene blue and crystal violet concentration in the analyzed samples. This novel method has a potential to be a useful semiquantitative determination procedure for dye analysis.

Gold nanorods assisted silver mirror reaction for consecutive color change based on-site visual semi-quantification of indoor formaldehyde

In the present study, a multicolor conversion strategy based on gold nanorods (AuNRs) assisted silver mirror reaction is developed for visual quantification of formaldehyde (HCHO). The method involves the silver deposition on the surface of AuNRs via the reduction reaction of Tollens' reagent in the presence of HCHO. The peak shifts of the longitudinal localized surface plasmon resonance (LSPR) and color variations of AuNRs solution are sensitive to the thickness of silver layer deposited on the surface of AuNRs. Under the optimized conditions, there is a good linear relationship between the peak shift and the concentration of HCHO (for both liquid sample and gas sample) in a wide range of concentration, thus an AuNRs based colorimetric assay for quantitative analysis of HCHO is established. Moreover, a series of consecutive color changes (from mauve to dusty blue, nattier blue, blue, mazarine blue, dark green, clay bank and finally orange red) responding to the presence and amount of HCHO enables visual semi-quantitative determination of HCHO within 15 min, and the clearly discernible dosage scale is as low as 0.10 μM. This assay exhibits desirable selectivity for HCHO over several common interfering organic molecular species and potential gas interferents, which has been successfully applied to measure the concentration of HCHO indoor.

Development of an LC-MS method for the semiquantitative determination of polyamide 6 contaminations in polyolefin recyclates

Recycling will be of increasing importance in the future, especially for plastic packaging waste mainly consisting of polyolefins. One major problem of recyclates comprises impurities which can have a significant negative impact on future product properties. Polyamide 6 can be found widely as contaminant in recycled polyolefins, leading to a need of quantification methods thereof. In this paper, a method development for the quantitative analysis of polyamide 6 is presented based on analysing ε-caprolactam and related cyclic oligomers as marker compounds in model recyclates of high- and low-density polyethylene and polypropylene compounded with low amounts of polyamide 6. For the method development and tentative identification of the different cyclic compounds, a HPLC-QTOF-MS was used and it was possible to detect six different compounds, ε-caprolactam and the corresponding cyclic di- to hexamer. The quantification was performed with a HPLC-QQQ-MS, equipped with a HILIC column, after sample preparation via microwave-assisted extraction. It could be shown that a good linearity from 0.2 up to 5 wt% polyamide 6 in the different polyolefins can be achieved. The cyclic trimer and tetramer show a low limit of quantification and are therefore well-suited for the quantification, whereas the other cyclic compounds can be then used as qualifiers to avoid false positives. To guarantee the applicability of the method, six real recyclate materials were analysed, whereby in three of them low amounts of polyamide 6 could be detected.Graphical abstract

Characterization of Gray-Black Stone Pillars of the Achaemenid Palace of Charkhab Borazja

Characterization of Gray-Black Stone Pillars of the Achaemenid Palace of Charkhab Borazja

Molecularly imprinted polymer-based device for field collection of oral fluid samples for cocaine identification

In this paper, a low–cost, rapid, easy, and potentially portable tool for the identification of cocaine and its semi-quantitative determination in oral fluid has been proposed. A field collection device has been designed, based on a cotton pad with an indicator and a molecularly imprinted polymer (MIP) sorbent, to selective retain cocaine from oral fluid components. After sample collection, cocaine is transferred by using phosphate buffer to the MIP and then eluted with 2-propanol. The obtained extract is analysed by ion mobility spectrometry (IMS), providing a cut-off value of 20 µg L−1 that identifies 100 % true-positive and 95 % true-negative samples. The MIP-IMS procedure has been validated by the analysis of oral fluid samples, collected from cocaine users at recreation environments, by comparing the results with lateral flow immunoassay and chromatographic reference methods. Thus, the proposed methodology allows a simple and fast cocaine identification that can be carried out in field by non-specialized personnel, such as health personnel, law enforcement bodies, and customs staff.

A unified design allows fine-tuning of biosensor parameters and application across bacterial species

In recent years, transcriptional biosensors have become valuable tools in metabolic engineering as they allow semiquantitative determination of metabolites in single cells. Although being perfectly suitable tools for high-throughput screenings, application of transcriptional biosensors is often limited by the intrinsic characteristics of the individual sensor components and their interplay. In addition, biosensors often fail to work properly in heterologous host systems due to signal saturation at low intracellular metabolite concentrations, which typically limits their use in high-level producer strains at advanced engineering stages.We here introduce a biosensor design, which allows fine-tuning of important sensor parameters and restores the sensor response in a heterologous expression host. As a key feature of our design, the regulator activity is controlled through the expression level of the respective gene by different (synthetic) constitutive promoters selected for the used expression host. In this context, we constructed biosensors responding to basic amino acids or ring-hydroxylated phenylpropanoids for applications in Corynebacterium glutamicum and Escherichia coli. Detailed characterization of these biosensors in liquid cultures and during single-cell analysis using flow cytometry showed that the presented sensor design enables customization of important biosensor parameters as well as application of these sensors in relevant heterologous hosts.

Rapid determination of pharmaceuticals in wastewater by direct infusion HRMS using target and suspect screening analysis

A wide-scope screening of active pharmaceutical ingredients (APIs) and their transformation products (TPs) in wastewater can yield valuable insights and pinpoint emerging contaminants that have not been previously reported. Such information is relevant to investigate their occurrence and fate in various environmental compartments. In this study, we explored the applicability of direct infusion high resolution mass spectrometry (DI-HRMS) for comprehensive and rapid detection of APIs and their TPs in wastewater samples. The method was developed using a Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) system and incorporated both wide-scope suspect screening and semi-quantitative determination of selected analytes. The identification strategy was based on the following criteria: narrow accurate mass window (±1.25 ppm) for two most abundant full-MS signals, isotopic pattern fit and additional confirmation on the basis of MS2 spectra at three fragmentation levels. The tentative identification of suspects and target compounds relied on an in-house database containing more than 500 different APIs and TPs. The measured fragment spectra were matched against experimental MS2 patterns obtained from a publicly available spectral library (MassBank of North America) and in-silico generated fragmentation features (from the CFM-ID algorithm). In total, 79 suspects were identified and 24 target compounds were semi-quantified in 72 wastewater samples. The highest detection frequencies in treated wastewater effluents were observed for diclofenac, metoprolol and telmisartan, while hydroxydiclofenac, dextrorphan, and carbamazepine metabolites were the most frequently detected TPs. The obtained API profiles were in accordance with the national consumption statistics and the origin of wastewater samples. The developed method is suitable for rapid screening of APIs in wastewater and can be used as a complementary tool to characterize API emissions from wastewater treatment facilities and to identify problematic compounds that require more rigorous monitoring.

Vitamins determination by TLC/HPTLC—a mini-review

This review describes the application of thin-layer chromatography (TLC) and high-performance thin-layer chromatography (HPTLC) in the separation and identification of vitamins from their mixtures using different kinds of mobile phases such as isocratic and mixed solvents as well as mobile phases containing various modifiers. TLC has long been used for the separation and semiquantitative determination of biomolecules including vitamins. HPTLC is the modified version of TLC, and it offers the advantages of better resolution, smaller sample size, and lesser volumes of mobile phases. In recent years, the emergence of advanced and fully automated chromatographic techniques such as high-performance liquid chromatography (HPLC) and gas chromatography (GC) has reduced the application of TLC/HPTLC for vitamins analysis. However, due to the inherent simplicity and cost-effectiveness, both TLC and HPTLC continue to be the methods of choice in small laboratories of developing countries. In this short review, the literature survey on TLC/HPTLC of vitamins covering the period 2011‒2019 has been encapsulated in a tabular form.

Pathology of bone epiphyses and frequency of various damage degree cases in patients with rheumatoid arthritis complicated by knee joint frontal deformities

Aim: based on several semi-quantitative morphometric indices, which represent pathological changes in femoral and tibial condyles, to determine pathological changes occurrence frequencies of damaged knee joints, complicated by frontal deformations. Materials and methods. Resected femoral and tibial condyles, obtained during knee replacement in 38 patients with rheumatoid arthritis and deformations of knee joints in frontal plane, served as material of current study. The following research methods were used: clinical examination, histological with semi-quantitative morphometric indices determination; statistical with determination of mean parameters, frequency of occurrence of cases with different gradations of indicators expression and their differences. Results. Groups of rheumatoid arthritis patients with lesions of knee joints complicated by deformities in frontal plane of different forms (valgus – varus), had significant differences by several clinical and clinical-visual indices. Pathological changes of epiphyses which are reflected by such morphometric parameters as “pannus structure and inflammation”, “inflammatory activity in subchondral spongiosa” and “stage of dystrophic-destructive changes of the joint surface” with different frequency and severity occur in the tissues of all rheumatoid arthritis patients with knee injuries, complicated by frontal deformations. In condyles from bones of one type, that form knee joint, compared in varus and valgus deformities, occurrence frequency of varying severity cases of separate morphometric indices varies in condyles according to different degree of compression. In condyles from bones of one type, which form knee joint, compared in different bones (femur and tibia) in cases of valgus deformity there was higher occurrence frequency of cases with more expressed indicator of “pannus structure and inflammation” in tibial condyles, in cases of varus deformity – in femoral condyles (independent of degree of compression). Conclusions. Results of study showed that degree of both clinical and morphometric indices of tibia and femur condyles condition in patients with rheumatoid arthritis and knee joint frontal deformities has no constant, unambiguous tendencies, and occurrence frequencies of cases with high and low degrees vary in wide limits.