Simultaneous Determination of Caffeine and Paracetamol in Commercial Formulations Using Greener Normal-Phase and Reversed-Phase HPTLC Methods: A Contrast of Validation Parameters

There has been no assessment of the greenness of the described analytical techniques for the simultaneous determination (SMD) of caffeine and paracetamol. As a result, in comparison to the greener normal-phase high-performance thin-layer chromatography (HPTLC) technique, this research was conducted to develop a rapid, sensitive, and greener reversed-phase HPTLC approach for the SMD of caffeine and paracetamol in commercial formulations. The greenness of both techniques was calculated using the AGREE method. For the SMD of caffeine and paracetamol, the greener normal-phase and reversed-phase HPTLC methods were linear in the 50–500 ng/band and 25–800 ng/band ranges, respectively. For the SMD of caffeine and paracetamol, the greener reversed-phase HPTLC approach was more sensitive, accurate, precise, and robust than the greener normal-phase HPTLC technique. For the SMD of caffeine paracetamol in commercial PANEXT and SAFEXT tablets, the greener reversed-phase HPTLC technique was superior to the greener normal-phase HPTLC approach. The AGREE scores for the greener normal-phase and reversed-phase HPTLC approaches were estimated as 0.81 and 0.83, respectively, indicated excellent greenness profiles for both analytical approaches. The greener reversed-phase HPTLC approach is judged superior to the greener normal-phase HPTLC approach based on numerous validation parameters and pharmaceutical assays.

Enantiomeric Separation and Molecular Modelling of Bioactive 4-aryl-3,4-dihydropyrimidin-2(1H)-one Ester Derivatives on Teicoplanin-Based Chiral Stationary Phase

The enantiomeric separation of 15 racemic 4-aryl-3,4-dihydropyrimidin-2(1H)-one (DHP) alkoxycarbonyl esters, some of which proved to be highly active as A2B adenosine receptor antagonists, was carried out by HPLC on ChirobioticTM TAG, a chiral stationary phase (CSP) bearing teicoplanin aglycone (TAG) as the chiral selector. The racemic compounds were separated under polar organic (PO) conditions. Preliminarily, the same selectands were investigated on three different Pirkle-type CSPs in normal-phase (NP) conditions. A baseline separation was successfully obtained on TAG-based CSPs for the majority of compounds, some of which achieved high enantioselectivity ratios (α > 2) in contrast with the smaller α values (1–1.5) and the lack of baseline resolution observed with the Pirkle-type CSPs. In particular, the racemic tetrazole-fused DHP ester derivatives, namely compounds 8 and 9, were separated on TAG-based HPLC columns with noteworthy α values (8.8 and 6.0, respectively), demonstrating the potential of the method for preparative purposes. A competition experiment, carried out with a racemic analyte (6) by adding N-acetyl-d-alanine (NADA) to the mobile phase, suggested that H-bonding interactions involved in the recognition of the natural dipeptide ligand d-Ala-d-Ala into the TAG cleft should be critical for enantioselective recognition of 4-aryl DHPs by TAG. The X-ray crystal structure of TAG was elucidated at a 0.77 Å resolution, whereas the calculation of molecular descriptors of size, polar, and H-bond interactions, were complemented with molecular docking and molecular dynamics calculations, shedding light on repulsive (steric effects) and attractive (H-bond—polar and apolar) interactions between 4-aryl DHP selectands and TAG chiral selectors.

The Separation of Cannabinoids on Sub-2 µm Immobilized Polysaccharide Chiral Stationary Phases

The increased use and applicability of Cannabis and Cannabis-derived products has skyrocketed over the last 5 years. With more and more governing bodies moving toward medical and recreational legalization, the need for robust and reliable analytical testing methods is also growing. While many stationary phases and methods have been developed for this sort of analysis, chiral stationary phases (CSPs) are unique in this area; not only can they serve their traditional chiral separation role, but they can also be used to perform achiral separations. Given that mixtures of cannabinoids routinely contain enantiomers, diastereomers, and structural isomers, this offers an advantage over the strictly achiral-only analyses. This work presents the separation of a 10-cannabinoid mixture on several polysaccharide-based sub-2 µm CSPs with both normal-phase and reversed-phase ultra-high-performance liquid chromatography (UHPLC) conditions. Along with the separation of the mixture, appropriate single-peak identification was performed to determine the elution order and reported where applicable.

Casimir Effect between Superconducting Plates in the Mixed State

The Casimir effect between type-II superconducting plates in the coexisting phase of a superconducting phase and a normal phase is investigated. The dependence of the optical conductivity of the superconducting plates on the external magnetic field is described in terms of the penetration depth of the incident electromagnetic field, and the permittivity along the imaginary axis is represented by a linear combination of the permittivities for the plasma model and Drude models. The characteristic frequency in each model is determined using the force parameters for the motion of the magnetic field vortices. The Casimir force between parallel YBCO plates in the mixed state is calculated, and the dependence on the applied magnetic field and temperature is considered.

Analysis of the Heterogeneities of First and Second Order of Cellulose Derivatives: A Complex Challenge

The complexity of the substituent distribution in polysaccharide derivatives is discussed and defined. The challenges regarding analytical characterization that results from various interrelated categories of distributions, including molecular weight, chemical composition, and microstructure, are outlined. Due to these convoluted levels of complexity, results should always be interpreted with carefulness. Various analytical approaches which have been applied to starch and cellulose derivatives are recapped, including enzymatic, mass spectrometric, and chromatographic methods. The relation of heterogeneities of first and second order among and along the polysaccharide chains is addressed. Finally, examples of own analytical work on cellulose ethers are presented, including the MS analysis of methyl cellulose (MC) blends and fractionation studies of fully esterified MC, especially its 4-methoxybenzoates by gradient HPLC on normal phase. Preparative fractionation according to the degree of substitution (DS) allows follow-up analysis in order to get more detailed information on the substituent distribution in such sub-fractions.

HPTLC Fingerprint Authentication of Selected Sideritis spp. Using a Pharmacognostic Approach

The genus Sideritis (Lamiaceae) comprises around 150 species, of which many are popular herbal remedies in Mediterranean folk medicine. Already mentioned by Dioscorides and Theophrastus, the “ironwort” or “Greek mountain tea” has been receiving increased attention in recent years. A European Union herbal monograph and assessment report (HMPC) has been issued, covering the species Sideritis scardica, S. clandestina, S. raeseri, and S. syriaca. This study presents results of a first pharmacognostic examination of the botanical and phytochemical differences among and between these emerging commercial species, and other, less studied species. An HPTLC method is proposed for normal phase separation of the species; this means applying two mobile phases on silica plates and subsequent derivatization with natural product reagent (NP/PEG) for visualization of phenolic compounds and anisaldehyde for a broader detection. With the help of selected reference compounds, a system suitability test was established for proper chromatographic separation. The method was applied to specimens from botanical gardens and commercial raw material in order to test its suitability for differentiation and authentication. The HPTLC analysis also includes, for the first time, S. hyssopifolia and other less used Sideritis species. The results might enable the development of a validated phytochemical fingerprint authentication procedure for quality assurance of Sideritis herba.

The Urgency of Public Transportation in Terms of Supervision in Accordance with Health Protocols

The goal of this study was to ascertain the critical nature of public transportation under the supervision of a health protocol. During the COVID-19 pandemic's New Normal phase, the government issued an appeal addressing health procedures for individuals who are active in public spaces or who use public facilities. This protocol also applies to the public transportation industry, specifically the bus industry. Health rules for bus use must be strictly adhered to and monitored in order to prevent the virus from spreading. The health protocol is implemented to offer a sense of security for public bus riders without jeopardizing the quality of service. A series of laws limiting capacity and enforcing strict adherence to health protocols for all modes of public transportation

Rapid, Highly-Sensitive and Ecologically Greener Reversed-Phase/Normal-Phase HPTLC Technique with Univariate Calibration for the Determination of Trans-Resveratrol

The rapid, highly-sensitive and ecologically greener reversed-phase (RP)/normal-phase (NP) high-performance thin-layer chromatography (HPTLC) densitometric technique has been developed and validated for the determination of trans-resveratrol (TRV). The reversed-phase HPTLC-based analysis of TRV was performed using ethanol–water (65:35, v v−1) combination as the greener mobile phase, while, the normal-phase HPTLC-based estimation of TRV was performed using chloroform–methanol (85:15, v v−1) combination as the routine mobile phase. The TRV detection was carried out at 302 nm for RP/NP densitometric assay. The linearity was recorded as 10–1200 and 30–400 ng band−1 for RP and NP HPTLC techniques, respectively. The RP densitometric assay was observed as highly-sensitive, accurate, precise and robust for TRV detection in comparison with the NP densitometric assay. The contents of TRV in commercial formulation were recorded as 101.21% utilizing the RP densitometric assay, while, the contents of TRV in commercial formulation were found to be 91.64% utilizing the NP densitometric assay. The greener profile of RP/NP technique was obtained using the analytical GREEnness (AGREE) approach. The AGREE scales for RP and NP densitometric assays were estimated 0.75 and 0.48, respectively. The recorded AGREE scale for the RP densitometric assay indicated that this technique was highly green/the ecologically greener compared to the NP densitometric assay. After successful optimization of analytical conditions, validation parameters, AGREE scale and chromatography performance, the RP densitometric assay with univariate calibration was found to be better than the NP densitometric assay for the analysis of TRV.

Validation of enantioseparation and quantitation of an active metabolite of abrocitinib in human plasma

Aims: A chiral HPLC–MS/MS method for quantitation of an active metabolite (M2) of abrocitinib was validated in human plasma. Methods: Protein precipitation extraction and normal phase LC with baseline separation of five analytes (abrocitinib; isomeric metabolites M1, M2, M3 and M4) were achieved followed by mass spectrometric quantitation of M2 using positive-mode APCI. Results: With a 5–5000 ng/ml assay range using 100 μl K2EDTA aliquot, the assay provided short (17-min) runtime and robust separation up to approximately 330 injections on one column. Interday and intraday accuracy ranged from ‐6.80% to 13.4%; between-day and within-day precision was ≤10.4%. Conclusion: The method was used in multiple clinical studies, with excellent run passing rate and incurred sample reproducibility.