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Studies have been conducted to evaluate the genetic potential of cotton species and to develop disease and pest resistant cotton varieties from them. The significance of the level of leaf hairiness in the representatives of the Gossypium L. family in tolerance to sucking pests, spider mite, aphid, was studied. Resources were obtained to measure or qualitatively assess leaf hairiness, transfer the hairiness marker for pest tolerance into the genome of G. hirsutum L., and create cultivars with a combination of tolerance and economic traits. In the C2 plants of the combinations obtained by cross-breeding the wild-type ridges with twisting hairiness with the analyzer L-001 line, separation of the hairiness character was noted, its ratio was 3:1 according to the phenotype (1:2:1 according to the genotype). This separation in second-generation hybrids indicates that the feather shape trait is monogenic in nature.

The wider application of vibration machines (VM) with electromagnetic motors (EMVM) in various industries, including in vibration test benches for telecommunication devices and equipment has been studied in the paper. Difficulties associated with maintaining their productivity and efficiency at a given level are largely hindered. These factors mainly depend on the determination of the degree of influence of the nonlinearities of the input-output characteristics on the output values of the VM, the possibilities of tuning into the resonance mode, and the control of the output values while ensuring the energy-saving mode of operation of the EMVM. The mathematical model has been developed for a frequency-controlled EMVM taking into account the nonlinear dependencies of the characteristics of the elements, which makes it possible to determine the most accurate amplitude of oscillations of the EMVM working body when passing through resonance, observed with changes in the voltage frequency. The analysis of the physical processes of the influence of nonlinear elements of the electric circuit of the EMVM on the electromagnetic quantities and the derived analytical expressions of these nonlinearities, which make it possible to determine the harmonic composition of the current of the EMVM winding, are made. The system of vector control of the EMVM and the inclusion of a mathematical model of the engine into the control system have been developed, which will allow calculating the frequencies of free oscillations of the working body for tuning into the resonance mode.

In order to conduct model experimental studies of the mutual influence of electromagnetic and mechanical transient processes of starting up inertial vibration drives with an asynchronous motor, its mathematical model is being developed. The analytical dependence of the dynamic mechanical characteristics of the vibrator at various values of the rotor acceleration is determined. The mathematical model uses the dynamic mechanical characteristics of an induction motor as a torque.

The role of mass spectrometry (MS) has become more important in most application domains in recent years. Pharmaceutical analysis is specific due to its stringent regulation procedures, the need for good laboratory/manufacturing practices, and a large number of routine quality control analyses to be carried out. The role of MS is, therefore, very different throughout the whole drug development cycle. While it dominates within the drug discovery and development phase, in routine quality control, the role of MS is minor and indispensable only for selected applications. Moreover, its role is very different in the case of analysis of small molecule pharmaceuticals and biopharmaceuticals. Our review explains the role of current MS in the analysis of both small-molecule chemical drugs and biopharmaceuticals. Important features of MS-based technologies being implemented, method requirements, and related challenges are discussed. The differences in analytical procedures for small molecule pharmaceuticals and biopharmaceuticals are pointed out. While a single method or a small set of methods is usually sufficient for quality control in the case of small molecule pharmaceuticals and MS is often not indispensable, a large panel of methods including extensive use of MS must be used for quality control of biopharmaceuticals. Finally, expected development and future trends are outlined., (© 2023 The Authors. Mass Spectrometry Reviews published by John Wiley & Sons Ltd.)

Two new ultra-high performance liquid chromatography (UHPLC) methods for analyzing 21 selected antivirals and their metabolites were optimized, including sample preparation step, LC separation conditions, and tandem mass spectrometry detection. Micro-solid phase extraction in pipette tips was used to extract antivirals from the biological material of Hanks balanced salt medium of pH 7.4 and 6.5. These media were used in experiments to evaluate the membrane transport of antiviral drugs. Challenging diversity of physicochemical properties was overcome using combined sorbent composed of C 18 and ion exchange moiety, which finally allowed to cover the whole range of tested antivirals. For separation, reversed-phase (RP) chromatography and hydrophilic interaction liquid chromatography (HILIC), were optimized using extensive screening of stationary and mobile phase combinations. Optimized RP-UHPLC separation was carried out using BEH Shield RP18 stationary phase and gradient elution with 25 mmol/L formic acid in acetonitrile and in water. HILIC separation was accomplished with a Cortecs HILIC column and gradient elution with 25 mmol/L ammonium formate pH 3 and acetonitrile. Tandem mass spectrometry (MS/MS) conditions were optimized in both chromatographic modes, but obtained results revealed only a little difference in parameters of capillary voltage and cone voltage. While RP-UHPLC-MS/MS exhibited superior separation selectivity, HILIC-UHPLC-MS/MS has shown substantially higher sensitivity of two orders of magnitude for many compounds. Method validation results indicated that HILIC mode was more suitable for multianalyte methods. Despite better separation selectivity achieved in RP-UHPLC-MS/MS, the matrix effects were noticed while using both chromatographic modes leading to signal enhancement in RP and signal suppression in HILIC.

In our previous study we proposed a screening approach using ultra-high performance supercritical fluid chromatography for the determination of 10 pharmaceutical quality control mixtures. Most of resulting methods offered baseline separation of all analytes. However, some of these methods had to be further optimized to ensure their successful validation and applicability to impurity control in drug substance and drug products. Several challenges occurred during the optimization including: (i) the necessity of the resolution of active pharmaceutical ingredient and following impurity equaling at least 3, which was especially difficult to achieve for mixtures of structurally close compounds, (ii) unrepeatable elution of compounds eluting close to the dead volume or at the end of the gradient elution, and (iii) shifts in retention times due to the column aging and effects of additive. The most frequent optimization adjustments involved changes in gradient program. Other adjustments such as the substitution of Viridis UPC 2 HSS C18 SB column with a slightly different Acquity UPLC HSS C18 SB column, the addition of acetonitrile in the modifier, and the column coupling also led to beneficial changes in selectivity. Subsequently, validation of all 10 methods was carried out to prove the applicability of ultra-high performance supercritical fluid chromatography methods for the impurity control in pharmaceuticals. Parameters recommended by ICH guidelines Q2 and Q3 including specificity, linearity, range, lower and upper limit of quantification, limit of detection, accuracy, and precision were examined. In addition, intermediate precision and the accuracy profiles were determined for selected methods. Overall, only two impurities did not meet the validation criteria due to low resolution and low sensitivity, respectively. Only identification threshold and not reporting threshold was met for this impurity., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier B.V. All rights reserved.)

Negative-ion hydrophilic liquid chromatography-electrospray ionization mass spectrometry (HILIC/ESI-MS) method has been optimized for the quantitative analysis of ganglioside (GM3) and other polar lipid classes, such as sulfohexosylceramides (SulfoHexCer), sulfodihexosylceramides (SulfoHex2Cer), phosphatidylglycerols (PG), phosphatidylinositols (PI), lysophosphatidylinositols (LPI), and phosphatidylserines (PS). The method is fully validated for the quantitation of the studied lipids in kidney normal and tumor tissues of renal cell carcinoma (RCC) patients based on the lipid class separation and the coelution of lipid class internal standard with the species from the same lipid class. The raw data are semi-automatically processed using our software LipidQuant and statistically evaluated using multivariate data analysis (MDA) methods, which allows the complete differentiation of both groups with 100% specificity and sensitivity. In total, 21 GM3, 28 SulfoHexCer, 26 SulfoHex2Cer, 10 PG, 19 PI, 4 LPI, and 7 PS are determined in the aqueous phase of lipidomic extracts from kidney tumor tissue samples and surrounding normal tissue samples of 20 RCC patients. S-plots allow the identification of most upregulated (PI 40:5, PI 40:4, GM3 34:1, and GM3 42:2) and most downregulated (PI 32:0, PI 34:0, PS 36:4, and LPI 16:0) lipids, which are primarily responsible for the differentiation of tumor and normal groups. Another confirmation of most dysregulated lipids is performed by the calculation of fold changes together with T and p values to highlight their statistical significance. The comparison of HILIC/ESI-MS data and matrix-assisted laser desorption/ionization mass spectrometric imaging (MALDI-MSI) data confirms that lipid dysregulation patterns are similar for both methods. Graphical abstract ᅟ.

Lipidomic analysis of biological samples in a clinical research represents challenging task for analytical methods given by the large number of samples and their extreme complexity. In this work, we compare direct infusion (DI) and chromatography - mass spectrometry (MS) lipidomic approaches represented by three analytical methods in terms of comprehensiveness, sample throughput, and validation results for the lipidomic analysis of biological samples represented by tumor tissue, surrounding normal tissue, plasma, and erythrocytes of kidney cancer patients. Methods are compared in one laboratory using the identical analytical protocol to ensure comparable conditions. Ultrahigh-performance liquid chromatography/MS (UHPLC/MS) method in hydrophilic interaction liquid chromatography mode and DI-MS method are used for this comparison as the most widely used methods for the lipidomic analysis together with ultrahigh-performance supercritical fluid chromatography/MS (UHPSFC/MS) method showing promising results in metabolomics analyses. The nontargeted analysis of pooled samples is performed using all tested methods and 610 lipid species within 23 lipid classes are identified. DI method provides the most comprehensive results due to identification of some polar lipid classes, which are not identified by UHPLC and UHPSFC methods. On the other hand, UHPSFC method provides an excellent sensitivity for less polar lipid classes and the highest sample throughput within 10min method time. The sample consumption of DI method is 125 times higher than for other methods, while only 40μL of organic solvent is used for one sample analysis compared to 3.5mL and 4.9mL in case of UHPLC and UHPSFC methods, respectively. Methods are validated for the quantitative lipidomic analysis of plasma samples with one internal standard for each lipid class. Results show applicability of all tested methods for the lipidomic analysis of biological samples depending on the analysis requirements., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Matrix-assisted laser desorption/ionization coupled with Orbitrap mass spectrometry (MALDI-Orbitrap-MS) is used for the clinical study of patients with renal cell carcinoma (RCC), as the most common type of kidney cancer. Significant changes in sulfoglycosphingolipid abundances between tumor and autologous normal kidney tissues are observed. First, sulfoglycosphingolipid species in studied RCC samples are identified using high mass accuracy full scan and tandem mass spectra. Subsequently, optimization, method validation, and statistical evaluation of MALDI-MS data for 158 tissues of 80 patients are discussed. More than 120 sulfoglycosphingolipids containing one to five hexosyl units are identified in human RCC samples based on the systematic study of their fragmentation behavior. Many of them are recorded here for the first time. Multivariate data analysis (MDA) methods, i.e., unsupervised principal component analysis (PCA) and supervised orthogonal partial least square discriminant analysis (OPLS-DA), are used for the visualization of differences between normal and tumor samples to reveal the most up- and downregulated lipids in tumor tissues. Obtained results are closely correlated with MALDI mass spectrometry imaging (MSI) and histologic staining. Important steps of the present MALDI-Orbitrap-MS approach are also discussed, such as the selection of best matrix, correct normalization, validation for semiquantitative study, and problems with possible isobaric interferences on closed masses in full scan mass spectra. Graphical Abstract ᅟ.

A novel and rapid sample pretreatment technique based on a combination of ultracentrifugation and solid-phase extraction for the determination of α-tocopherol in human erythrocyte membranes by high-performance liquid chromatography with ultraviolet detection is presented in this work. Red blood cell samples were ultracentrifuged (288 000 × g, 3 min, 4°C) in the presence of d-mannitol, 4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid and calcium chloride. The α-tocopherol was then extracted from the erythrocyte membranes by solid-phase extraction with n-hexane in the presence of ascorbic acid. Tocopherol acetate was used as the internal standard. The extract was dissolved in methanol and separated on the monolithic column Chromolith Performance RP-18e (100 × 4.6 mm) using 100% methanol as the mobile phase. The absorbance of α-tocopherol was measured at a wavelength of 295 nm. The method was validated and showed sufficient accuracy and precision, ranging from 96.4 to 100.8% and from 4.5 to 6.3%, respectively. Moreover, the developed method was applied to the determination of erythrocyte α-tocopherol in real samples from patients. The combined ultracentrifugation and solid-phase extraction technique substantially decreased the time for the sample pretreatment step compared to liquid-liquid extraction and could be applicable for the quantitation of other analytes in erythrocyte membranes., (© 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)