Analytica, Volume 3, Issue 2 (June 2022) – 7 articles

Benzodiazepines (BZDs) are one of the most important drugs that have been used in the treatment of neuropsychological disorders. Indeed, BZDs are abused by drug addicts regardless of their therapeutic uses. Therefore, it was important in forensic and clinical toxicology to reach an easy and reliable method for the screening and quantification of BZDs in the human plasma matrix. In the current work, five BZDs, namely bromazepam, clonazepam, lorazepam, nordiazepam and diazepam were simultaneously separated and detected by a simple and reliable RPLC method in a human plasma matrix. Isocratic mobile elution consisting of 20 mmol L⁻¹ phosphate buffer (pH 7.0) and methanol (50:50, v/v) on a Symmetry C18 column was employed. The flow rate, wavelength and column temperature were fixed at 1.0 mL min⁻¹, 214 nm and 40 °C, respectively. The proposed method was validated, giving a linearity within the concentration ranges 5–500 ng mL⁻¹ for bromazepam and diazepam, 3–500 ng mL⁻¹ for clonazepam and lorazepam and 1–500 ng mL⁻¹ for nordiazepam with a determination coefficient (R²) more than 0.9992. The LOD values for the selected BZDs ranged from 0.54 to 2.32 and from 1.78 to 7.65 ng mL⁻¹ for standard methanolic and plasma matrices, respectively. Precision, accuracy, selectivity, stability, and robustness were some of the terms considered in validating the current RPLC method. Based on these results, a simple and reliable RPLC method was successfully applied to quantify BZDs in human plasma matrix appearing with recoveries ranging from 96.5 to 107.5% and interday RSD less than 4%. The current developed method was useful for rapidly screening the most commonly used BZDs in the market within their therapeutic concentration ranges. Full article

Ionic liquids are a very important class of compounds due to their remarkable properties and wide range of applications. On the other hand, capillary electrophoresis is also gaining importance in separation science because of its fast speed and inexpensive nature. The use of ionic liquids in capillary electrophoresis is gaining importance continuously. The present review article describes the applications of ionic liquids in capillary electrophoresis. This article also describes the general aspects of ionic liquids and capillary electrophoresis. The use of ionic liquids in capillary electrophoresis, optimization of separation, mechanism of separation, and toxicity of ionic liquids, as well as their future perspectives, have also been discussed. It was observed that not much work has been performed in capillary electrophoresis using ionic liquids. It was also realized that the use of ionic liquids in capillary electrophoresis could revolutionize analytical science. Briefly, there is a great need for the use of ionic liquids in capillary electrophoresis for better and more effective separation. Full article

We determined the antifungal and antimicrobial sensitivity of Euphorbia tirucalli extracts in vitro. Antifungal and antibacterial activity was determined based on the M38-A and M26-A protocols, respectively. The methanolic and ethanolic partitions demonstrated antidermatophytic activity against Trichophyton rubrum (MIC 125 µg/mL for ethanol and MIC 125 µg/mL for methanol) and T. interdigitalis (MIC 500 µg/mL for ethanol; 125 µg/mL for methanol). These partitions also showed antibacterial activity—the ethanolic partition had an MIC of 1.56 ± 0.02 mg/mL against methicillin-resistant Staphylococcus aureus (clinical isolate), 6.25 ± 0.04 mg/mL against Staphylococcus aureus BAA-44, 3.13 ± 0.13 mg/mL against Pseudomonas aeruginosa 27853, and 3.13 ± 0.15 mg/mL against Escherichia coli ATCC 25922; the methanolic partition showed an MIC of 1.56 ± 0.02 mg/mL against P. aeruginosa 27853 and 1.56 ± 0.043 mg/mL against E. coli ATCC 25922. These partitions show promise as antimicrobial agents or adjuvants in the treatment of infections caused by these microorganisms. Full article

In this study, a simple, fast, and effective methodology has been developed for the detection and quantification of seven phthalates potentially released in hot drinks from disposable containers used in vending machines. The authors determined the optimal conditions to be applied during the various steps of extraction of seven phthalates (DMP, DEP, DBP, DiBP, DEHP, DNOP, and DDP) from hot beverages using a model solution. The extraction and preconcentration technique used was ultrasound–vortex-assisted dispersive liquid–liquid microextraction (UVA-DLLME) followed by gas chromatographic analysis obtaining recoveries from 66.7% to 101.2% with precision and reproducibility <6.3% and <11.1%, respectively. The influence of waiting time, from the dispensing of the drink to its actual consumption, for the extraction of molecules was investigated, obtaining a temporal release profile slightly shifted towards the PAEs with higher molecular weight and vice versa for those with low molecular weight. In addition, the best instrumental parameters to be applied during the analysis of the extracts obtained were established. This optimization was carried out using GC-FID, whereas the analysis of real samples was carried out by means of GC-IT/MS for ultra-trace analysis purposes; limits of detection (LODs) ranging between 0.8 ng mL⁻¹ and 15.4 ng mL⁻¹ and limits of quantification (LOQs) from 1.6 ng mL⁻¹ to 35.8 ng mL⁻¹, both of them lower than those found by FID, were obtained. Full article

The removal of contaminants of emerging concern (CECs) occurring in wastewater effluents, such as pharmaceutically active substances (PhACs) and personal care products, pose a big research challenge since they can be a major source of pollution for water bodies and a danger to public health. The objective of this work was to perform a comprehensive monitoring of a broad set of PhACs (>130) in a wastewater treatment plant (WWTP) close to Thessaloniki (Greece), as well as to evaluate the potential of heterogeneous catalytic ozonation for the removal of CECs from wastewater through a continuous flow system. The high-resolution mass spectrometry analysis revealed the highest average concentrations for irbesartan (1817 ng/L). Antihypertensives along with antibiotics, psychiatrics, and β-blockers were found to aggravate the effluents. Removal efficiency after conventional treatment was >30%. The results from catalytic ozonation unit operation indicate that the introduction of a proper solid material that acts as catalyst can enhance the removal of CECs. A preliminary risk assessment using the risk quotient (RQ) revealed that irbesartan and telmisartan entail high acute risk. The overall results underline the urgent need to incessantly monitor PhACs and expand the toxicological studies to establish the sublethal and chronic effects on aquatic organisms. Full article

Sweat is a potential biological fluid for the non-invasive analytical assessment of diverse molecules, including biomarkers. Notwithstanding, the sampling methodology is critical, and it must be assessed prior to using sweat for clinical diagnosis. In the current work, the analytical methodology was further developed taking into account the sampling step, in view of the identification and level variations of sweat components that have potential to be stress biomarkers using separation by liquid chromatography and detection by tandem mass spectrometry, in order to attain a screening profile of 26 molecules in just one stage. As such, the molecule identification was used as a test for the evaluation of the sampling procedures, including the location on the body, using patches for long-term sampling and vials for direct sampling, through a qualitative approach. From this evaluation it was possible to conclude that the sampling may be performed on the chest or back skin. Additionally, possible interference was evaluated. The long-term sampling with patches can be used under both rest and exercise conditions with variation of the detected molecule’s levels. The direct sampling, using vials, has the advantage of not having interferences but the disadvantage of only being effective after exercise in order to have enough sample for sweat analysis. Full article

Nonsteroidal anti-inflammatory drugs are the most commonly prescribed anti-inflammatory drugs worldwide. The most common side effects are gastrointestinal. Pantoprazole, a proton pump inhibitor (PPI), can be used to prevent these events from occurring. In this study, we attempt to develop and validate a novel method for determining and validating the fixed-dose combination of meloxicam and pantoprazole. A new method has been developed and validated to estimate pantoprazole and meloxicam in a fixed-dose combination using RP-HPLC. In order to separate the drugs, a mobile phase phosphate buffer/acetate was used (30:70, v/v), with a pH of 3.4 and a flow rate of 1.0 mL/min at 25 °C. The detection wavelength for the drugs was at a wavelength of 310 nm. The retention times for meloxicam and pantoprazole were 6 and 9 min, respectively. In concentrations ranging from 0.1 to 200 mg/L, the linearity of the detector was established. The r was 0.9998 for both drugs. Recovery rates ranged from 98 to 102% on average. According to the guidelines of the International Council on Harmonization, the results were satisfactory. Using the method presented herein, the pharmaceutical formulation of the combined meloxicam and pantoprazole can be routinely tested. Full article