QCL Infrared Spectroscopy Combined with Machine Learning as a Useful Tool for Classifying Acetaminophen Tablets by Brand.

The development of new methods of identification of active pharmaceutical ingredients (API) is a subject of paramount importance for research centers, the pharmaceutical industry, and law enforcement agencies. Here, a system for identifying and classifying pharmaceutical tablets containing acetaminophen (AAP) by brand has been developed. In total, 15 tablets of 11 brands for a total of 165 samples were analyzed. Mid-infrared vibrational spectroscopy with multivariate analysis was employed. Quantum cascade lasers (QCLs) were used as mid-infrared sources. IR spectra in the spectral range 980-1600 cm-1 were recorded. Five different classification methods were used. First, a spectral search through correlation indices. Second, machine learning algorithms such as principal component analysis (PCA), support vector classification (SVC), decision tree classifier (DTC), and artificial neural network (ANN) were employed to classify tablets by brands. SNV and first derivative were used as preprocessing to improve the spectral information. Precision, recall, specificity, F1-score, and accuracy were used as criteria to evaluate the best SVC, DEE, and ANN classification models obtained. The IR spectra of the tablets show characteristic vibrational signals of AAP and other APIs present. Spectral classification by spectral search and PCA showed limitations in differentiating between brands, particularly for tablets containing AAP as the only API. Machine learning models, specifically SVC, achieved high accuracy in classifying AAP tablets according to their brand, even for brands containing only AAP.

A novel "ON-OFF-ON" colorimetric and fluorescence dual-signal sensing APAP based on TSPP-Fe3.

Acetaminophen, also known as paracetamol (APAP), is a commonly used over-the-counter medication that is often used to treat headaches, toothaches, joint pain, muscle pain, and to lower body temperature. However, overdose can lead to liver damage, gastrointestinal distress, kidney damage, and cardiovascular disease. Therefore, it is very important to establish a method to quickly detect APAP. A novel "ON-OFF-ON" colorimetric and fluorescence dual-signal sensing system was constructed for the quantitative detection of APAP based on 5,10,15,20-tetrakis(4-sulphonatophenyl) porphyrin (TSPP) dual-signal probe. The absorbance and fluorescence intensity of TSPP respectively were quenched when Fe3+ was introduced into TSPP solution. At this point, the color of the corresponding solution changed from red to green. The absorbance and fluorescence intensity of TSPP respectively were restored when APAP was added to the TSPP-Fe3+ system. At this time, the color of the solution changed from green to colorless. Therefore, an "ON-OFF-ON" dual-signal sensing study of APAP were constructed using TSPP as the colorimetric and fluorescent probe. The proposed colorimetric sensing system had a wide linear range in the 13.12 mM âˆ¼ 23.20 mM with 0.11 mM of limit of detection (LOD, S/N = 3). And the proposed fluorescence sensing system had a wide linear range in the 3.45 mM âˆ¼ 12.50 mM and 41.67 mM âˆ¼ 65.22 mM with 0.83 mM of limit of detection (LOD, S/N = 3). The dual-signal sensing system were applied to the APAP detection of real samples.

Continuous stationary phase gradient preparation on planar chromatographic media using vapor phase deposition of silane.

A new, versatile, and straightforward vapor phase deposition (VPD) approach was used to prepare continuous stationary phase gradients (cSPGs) on silica thin-layer chromatography (TLC) plates using phenyldimethylchlorosilane (PDCS) as a precursor. A mixture of paraffin oil and PDCS was placed at the bottom of an open-ended rectangular chamber, allowing the reactive silanes to evaporate and freely diffuse under a controlled atmosphere. As the volatile silane diffused across the length of the TLC plate, it reacted with the surface silanol groups thus functionalizing the surface in a gradient fashion. Characterization of the gradient TLC plates was done through UV visualization and diffuse reflectance spectroscopy (DRS). Visualizing the fluorescent gradient plates under UV radiation shows the clear presence of a gradient with the side closest to the vapor source undergoing the most modification. More quantitative characterization of the shape of the gradient was provided by DRS. The DRS showed that the degree of modification and shape of the gradient was dependent on the concentration of silane, VPD time, and relative humidity. To evaluate the chromatographic performance, a mixture of three aromatic compounds (acetaminophen (A), aspirin (As), and 3-hydroxy-2-naphthoic acid (3H)) was spotted on the high (GHP) and low phenyl (GLP) ends of the gradient TLC plates and the results compared to the separations carried out on unmodified and uniformly modified plates. The GHP TLC plates showed retention factors (Rf) of 0.060 ± 0.006, 0.391 ± 0.006, and 0.544 ± 0.006, whereas the unmodified plate displayed Rf values of 0.059 ± 0.006, 0.092 ± 0.003, and 0.037 ± 0.002 for the analytes A, As, and 3H, respectively. From the Rf values, it was observed that each modified plate exhibited different selectivity for the analytes. The GHP TLC plates exhibited better separation performance, and improved resolution compared to the GLP, unmodified, and uniformly modified plates. Overall, VPD is a new, cost-effective method for creating a gradient on the stationary phase which has the potential to advance chromatographic separation capabilities.

Development of an electrochemical sensor for the quantification of ascorbic acid and acetaminophen in pharmaceutical samples.

This work presents the modification of glassy carbon electrodes (GCE) by using a dispersion resulting from the non-covalent functionalization of multi-walled carbon nanotubes (MWCNT) with polyarginine (polyArg). MWCNT-polyArg is used for the quantification of ascorbic acid (AA) in the presence of acetaminophen (APAP) and viceversa. Since ascorbic acid and acetaminophen are strongly absorbed on GCE/MWCNT-polyArg, they can be detected in the presence of 4.0×10-5 M acetaminophen (and 3.0×10-5 M ascorbic acid) by using adsorptive stripping with media exchange and differential pulse voltammetry. Using water as the solvent for the MWCNT dispersion, the result was Z-potential of 0.053 ± 0.006 V. The developed sensor showed excellent specificity, sensitivity, stability and reproducibility compared to previously published sensors. The GCE/MWCNT-polyArg sensor shows a fast response time of ∼5 minutes, low limits of detection and quantification for AA (0.95 and 2.9 µM respectively) and APAP (0.27 and 0.82µM, respectively), high sensitivity of 0.0616 µA/M for AA or APAP 0.240µA/M. It was used to test its practicability by determining the concentration of AA or APAP (AA and APAP) in pharmaceutical samples. Finally, the simultaneous measurement of ascorbic acid and acetaminophen in pharmaceuticals showed a good correlation, with a maximum error and RSD of 4.5 and 5.1 %, respectively.

Synchronous analysis of acetaminophen, codeine, and caffeine in human fluids employing graphite screen-printed electrodes.

A facile electrochemical approach is proposed for the synchronous determination of acetaminophen (ACP), codeine (COD) and caffeine (CAF) utilizing unmodified screen-printed electrodes (SPEs). The determination of ACP, COD and CAF has been explored across different supporting electrolytes including sulfuric acid (H2SO4), hydrochloric acid (HCl), phosphoric acid (H3PO4) and Briton Robinson (B.R) buffer solutions. It was found that a 0.05 mol L-1 sulfuric acid solution is an optimal supporting electrolyte utilized for voltammetric analysis of ACP, COD, and CAF with improved sensitivity, stability, and reproducibility. The electro-analytical sensing of ACP, COD and CAF was investigated using SPEs within linear concentration ranges of 3.0-35.0 µmol L-1, 10-160 µmol L-1 and 10-160 µmol L-1 and revealed competitively low limits of detection (3S/N) of 0.9, 4.8 and 6.3 µmol L-1 for ACP, COD and CAF, respectively. The results indicated the possibility of such a simple and quick electroanalytical protocol for online monitoring of pharmaceutical formulations comprising ACP, COD, and CAF drugs in human fluids with satisfactory recovery.

Proving the automatic benchtop electrochemical station for the development of dopamine and paracetamol sensors.

The introduced work represents an implementation of the automatic benchtop electrochemical station (BES) as an effective tool for the possibilities of high-throughput preparation of modified sensor/biosensors, speeding up the development of the analytical method, and automation of the analytical procedure for the determination of paracetamol (PAR) and dopamine (DOP) as target analytes. Within the preparation of gold nanoparticles modified screen-printed carbon electrode (AuNPs-SPCE) by electrodeposition, the deposition potential EDEP, the deposition time tDEP, and the concentration of HAuCl4 were optimized and their influence was monitored on 1 mM [Ru(NH3)6]3+/2+ redox probe and 50 µM DOP. The morphology of the AuNPs-SPCE prepared at various modification conditions was observed by SEM. The analytical performance of the AuNPs-SPCE prepared at different modification conditions was evaluated by a construction of the calibration curves of DOP and PAR. SPCE and AuNPs-SPCE at modification condition providing the best sensitivity to PAR and DOP, were successfully used to determine PAR and DOP in tap water by "spike-recovery" approach. The BES yields better reproducibility of the preparation of AuNPs-SPCE (RSD = 3.0%) in comparison with the case when AuNPs-SPCE was prepared manually by highly skilled laboratory operator (RSD = 7.0%).

Optimization, kinetics, and pathways of pharmaceutical pollutant degradation using solar Fenton technique.

Solar Fenton is an important and extensively used advanced oxidation process (AOP) to degrade pharmaceutical pollutants. The objective of this study was to evaluate the performance of simultaneous degradation of the mixed pollutants (amoxicillin, acetaminophen, and ciprofloxacin) for an aqueous solution using the solar Fenton process. Operating parameters such as pH, iron doses, H2O2 doses, pollutant concentrations, and time were studied. From the experimental results, the ideal conditions were obtained for the removal of mixed pollutants such as pH 3, Fe2+ 0.04 mM, H2O2 4 mM, the concentration of the mixed pollutants 5 mg/L, solar radiation 400 W/m2, and time 10 min, respectively. The pseudo-first-order kinetics were utilized to investigate the degradation efficacy of the mixed pollutants. The result of the study indicates that the degradation efficiency was > 99% for the mixed pollutants. A maximum of 63% mineralization was observed, and hydroxyl radical scavenger effects were studied. The best optimal conditions were applied to assess the spiked wastewater (municipal wastewater (MWW) and hospital wastewater (HWW)). The highest elimination rates for AMX, ACET, and CIP were observed as 65%, 89%, and 85% for MWW and 76%, 92%, and 80% for HWW, respectively. The degraded by-products were detected by LC-ESI-MS in the water matrix (aqueous solution and spiked wastewater), and ECOSAR analysis was performed for the transformed products. The study concluded that the solar Fenton technique is promising and effective for the removal of mixed pollutants from the water matrix.

Corn-inspired high-density plasmonic metal-organic frameworks microneedles for enhanced SERS detection of acetaminophen.

Effective monitoring of acetaminophen (APAP) dosage is crucial for preventing antipyretic abuse, ensuring therapeutic efficacy, and minimizing toxic effects. However, existing self-monitoring methods are limited. In this study, we designed a plasmonic microneedle (MN) sensor for real-time nondestructive monitoring of acetaminophen levels in dermal interstitial fluid (ISF) by employing a handheld Raman spectrometer. The fabricated MN sensor incorporated a high-density plasmonic MOFs known as HDPM, which unique structure of large specific surface area, specific pore structure as well as high density gold nanospheres packing enabled the excellent performance of selective ISF drug enrichment and surface-enhanced Raman scattering (SERS). The maximum electric field enhancement factor of the HDPM nanostructure could be calculated as 5.73 × 107. The developed HDPM@MNs was characterized with a core-shell type "soft on the outside and rigid on the inside" structure, which exhibited sufficient hardness and flexibility to penetrate the dermal tissue with little damage, and robust SERS enhancement effect in APAP detection without any interfering peaks. Through a hydrogel drug simulation experiment, the sensor demonstrated robust capabilities for acetaminophen enrichment and monitoring, exhibiting excellent stability and repeatability. The quantitative detection window spanned from 1 to 100 µM, with a low detection limit reaching 0.45 µM. Furthermore, by monitoring the concentration of acetaminophen in the interstitial fluid of rat skin at different doses and for different administration times, the HDPM@MNs can be used to determine the pharmacokinetics of acetaminophen in rats and the physiological characteristics associated with various dosage regimens. This work not only holds promise for drug monitoring but also provides a novel approach for nondestructive monitoring of other crucial low-abundance physiological markers.

Development of Response Surface Approach for Determination of Paracetamol, Chlorpheniramine Maleate, Caffeine and Ascorbic Acid by Green HPLC Method: A Desirability-Based Optimization.

Design of experiment is an efficient and cost-effective tool to optimize the chromatographic separation of a multicomponent mixture. The central composite design was conducted to develop and optimize a green high performance liquid chromatography (HPLC) method for simultaneous quantitation of a quaternary mixture of paracetamol, chlorpheniramine maleate, caffeine and ascorbic acid in their pharmaceutical dosage form as well as the determination of their dissolution profile. A five-level three-factor model was performed to investigate the effect of mobile phase composition, pH and flow rate on enhanced resolution and short run time. Analysis was performed using a Kinitex EVO C18 column and a mobile phase composed of methanol: 0.02 M phosphate buffer pH 3.3 (34:66, v/v) at 1.0 mL/min using photodiode array detection. Optimum chromatographic separation was achieved in <6 min with a desirability of 0.999. Linearity was achieved over a range of 1.00-300.00, 1.00-50.00, 2.00-50.00 and 2.00-100.00 µg/mL for paracetamol, chlorpheniramine maleate, caffeine and ascorbic acid, respectively, with a limit of detection (<0.1 µg/mL). The greenness profile was evaluated using the analytical eco-scale and Analytical GREEnness Metric Approach with values of 81 and 0.77, respectively.

A miniaturized additive-manufactured carbon black/PLA electrochemical sensor for pharmaceuticals detection.

Additive manufacturing is a technique that allows the construction of prototypes and has evolved a lot in the last 20 years, innovating industrial fabrication processes in several areas. In chemistry, additive manufacturing has been used in several functionalities, such as microfluidic analytical devices, energy storage devices, and electrochemical sensors. Theophylline and paracetamol are important pharmaceutical drugs where overdosing can cause adverse effects, such as tachycardia, seizures, and even renal failure. Therefore, this paper aims at the development of miniaturized electrochemical sensors using 3D printing and polylactic acid-based conductive carbon black commercial filament for theophylline and paracetamol detection. Electrochemical characterizations of the proposed sensor were performed to prove the functionality of the device. Morphological characterizations were carried out, in which chemical treatment could change the surface structure, causing the improvement of the analytical signal. Thus, the detection of theophylline at a linear range of 5.00-150 µmol L-1 with a limit of detection of 1.2 µmol L-1 was attained, and the detection of paracetamol at a linear range of 1.00-200 µmol L-1 with a limit of detection of 0.370 µmol L-1 was obtained, demonstrating the proposed sensor effectively detected pharmaceutical drugs.

Detection of acetaminophen and P-aminophenol simultaneously by an electrochemical sensor based on Fe-NC derivatives attached with Ti3C2 QDs.

In this paper, Ti3C2 QDs and Fe-ZIF-8 were synthesized by a straightforward hydrothermal method. Fe-ZIF-8 was pyrolyzed at high temperatures to obtain Fe-nanoclusters (Fe-NC). Then Fe-NC is mixed with Ti3C2 QDs to form a new composite material (Ti3C2 QDs/Fe-NC), and its microstructure and composition were analyzed by technology. The proposed material can detect acetaminophen (PA) and P-aminophenol (4-AP) simultaneously with excellent detection performance. With the best conditions, the linear ranges and detection limits were 0.50-210.00 µM, 0.03 µM (S/N = 3) and 0.50-150.00 µM, 0.06 µM (S/N = 3) for PA and 4-AP, respectively. The sensor has lower detection limits and wider linear ranges, and can successfully detect 4-AP and PA in river water and acetaminophen tablets at the same time, showing potential practical application prospects. Especially, this study reports the modification of MOF derivatives with Ti3C2 QDs for the first time, which expands the application scope of Quantum Dots and MOF derivatives.

Development of a novel UPLC approach to co-prediction of four active compounds in a multi-component pharmaceutical preparation.

In this work, a new ultra-performance liquid chromatography method based on photodiode array detection (UPLC-PDA) was first developed for the quantitative analysis of the quaternary mixture of ascorbic acid (AA), paracetamol (PAR), caffeine (CAF) and chlorpheniramine maleate (CPA) in a commercial dosage form. The developed UPLC-PDA method offered a new possibility for the co-determination of four active ingredients in a drug combination with short run time and simple sample preparation. The successful chromatographic separation of the four drugs was performed using a Waters Acquity UPLC BEH C18 column (1.7 µm 2.1 × 100 mm) (Mildford, USA) and a mobile phase consisting of water (12 %), acetonitrile (13 %) and 0.1 M H3PO4 (75 %) at a flow rate of 0.25 mL/min. The validation of the proposed UPLC-PDA approach was verified by analyzing synthetic mixtures, inter- and intra-day experiments, and commercial powder samples and provided satisfactory results.

A Novel Low-Frequency Electromagnetic Active Inertial Sensor for Drug Detection.

The purpose of this paper is to demonstrate a new discovery regarding the interaction between materials and very low radio frequencies. Specifically, we observed a feedback response on an inertia active sensor when specific frequencies (around 2-4 kHz) are used to irradiate targeted pharmaceutical samples like aspirin or paracetamol drugs. The characteristics of this phenomenon, such as excitation and relaxation time, the relation between deceleration and a material's quantity, and signal amplitude, are presented and analyzed. Although the underlying physics of this phenomenon is not yet known, we have shown that it has potential applications in remote identification of compounds, detection, and location sensing, as well as identifying substances that exist in plants without the need for any processing. This method is fast, accurate, low-cost, non-destructive, and non-invasive, making it a valuable area for further research that could yield spectacular results in the future.

Anthraquinone/activated carbon electrochemical sensor and its application in acetaminophen analysis.

Acetaminophen (AC) can inhibit the synthesis of prostaglandins in the body, and has antipyretic and analgesic effects. In this paper, a two-step microwave impregnation method was used to prepare anthraquinone (AQ)-doped carbon composite, which were applied to the surface modification of glassy carbon electrodes (GCE) for the determination of acetaminophen (AC) using differential pulse voltammetry (DPV). The composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman and Fourier infrared spectroscopy (FT-IR). The results showed that anthraquinone was successfully modified on the surface of activated carbon. The peak current of AC increased with its concentration in the range of 0.1 µM to 700 µM (R2 = 0.998) and a detection limit of 0.05 µM was obtained with 20%AQ doped carbon electrochemical sensor (20%AQ-C/GCE). Electrochemical Impedance Spectroscopy (EIS) test results indicated that the charge transfer resistance (Rct) of 20%AQ-C/GCE is only the one-fourth of that of bare GCE. The proposed 20%AQ-C/GCE sensor has good stability, reproducibility and selectivity for the detection of AC. The sensor is also suitable for the detection of real samples, indicating its good practicality.

Circular economical approach of extracting nanocarbons from waste pea peel for sensing of p-nitrophenol and its conversion into paracetamol.

An important paradigm shift towards the circular economy is to prioritize waste prevention, reuse, recycling, and recovery before disposal is necessary. In this context, a sustainable protocol of converting waste pea peel (wPP) into low-cost carbon nanomaterials for sensing and conversion of p-nitrophenol (p-NP) into value-added paracetamol is being reported. Two fractions of the carbonaceous nanomaterials were obtained after the hydrothermal treatment (HT) of wPP, firstly an aqueous portion containing water-soluble carbon dots (wPP-CDs) and a solid residue, which was converted into carbonized biochar (wPP-BC). Blue-colored fluorescent wPP-CDs displayed excitation-dependent and pH-independent properties with a quantum yield (QY) of 8.82 %, which were exploited for the fluorescence sensing of p-NP with 4.20 µM limit of detection. Pyrolyzed biochar acting as an efficient catalyst effectively reduces p-NP to p-aminophenol (p-AP) in just 16 min with a 0.237 min-1 rate of conversion. Furthermore, the produced p-AP was converted into paracetamol, an analgesic and antipyretic drug, to achieve zero waste theory. Thus, this study provides the execution of sustainable approaches based on the integral valorization of biowaste that can be further recycled and reused, offering an effective way to attain a profitable circular economy.

Highly Sensitive Wearable Sensor Based on (001)-Orientated TiO2 for Real-Time Electrochemical Detection of Dopamine, Tyrosine, and Paracetamol.

The concentration of dopamine (DA) and tyrosine (Tyr) reflects the condition of patients with Parkinson's disease, whereas moderate paracetamol (PA) can help relieve their pain. Therefore, real-time measurements of these bioanalytes have important clinical implications for patients with Parkinson's disease. However, previous sensors suffer from either limited sensitivity or complex fabrication and integration processes. This work introduces a simple and cost-effective method to prepare high-quality, flexible titanium dioxide (TiO2) thin films with highly reactive (001)-facets. The as-fabricated TiO2 film supported by a carbon cloth electrode (i.e., TiO2-CC) allows excellent electrochemical specificity and sensitivity to DA (1.390 µA µM-1 cm-2), Tyr (0.126 µA µM-1 cm-2), and PA (0.0841 µA µM-1 cm-2). More importantly, accurate DA concentration in varied pH conditions can be obtained by decoupling them within a single differential pulse voltammetry measurement without additional sensing units. The TiO2-CC electrochemical sensor can be integrated into a smart diaper to detect the trace amount of DA or an integrated skin-interfaced patch with microfluidic sampling and wireless transmission units for real-time detection of the sweat Try and PA concentration. The wearable sensor based on TiO2-CC prepared by facile manufacturing methods holds great potential in the daily health monitoring and care of patients with neurological disorders.

Multi-walled carbon nanotubes/carbon black/rPLA for high-performance conductive additive manufacturing filament and the simultaneous detection of acetaminophen and phenylephrine.

The combination of multi-walled carbon nanotubes (MWCNT) and carbon black (CB) is presented to produce a high-performance electrically conductive recycled additive manufacturing filament. The filament and subsequent additively manufactured electrodes were characterised by TGA, XPS, Raman, and SEM and showed excellent low-temperature flexibility. The MWCNT/CB filament exhibited an improved electrochemical performance compared to an identical in-house produced bespoke filament using only CB. A heterogeneous electrochemical rate constant, [Formula: see text] of 1.71 (± 0.19) × 10-3 cm s-1 was obtained, showing an almost six times improvement over the commonly used commercial conductive CB/PLA. The filament was successfully tested for the simultaneous determination of acetaminophen and phenylephrine, producing linear ranges of 5-60 and 5-200 µM, sensitivities of 0.05 µA µM-1 and 0.14 µA µM-1, and limits of detection of 0.04 µM and 0.38 µM, respectively. A print-at-home device is presented where a removable lid comprised of rPLA can be placed onto a drinking vessel and the working, counter, and reference components made from our bespoke MWCNT/CB filament. The print-at-home device was successfully used to determine both compounds within real pharmaceutical products, with recoveries between 87 and 120% over a range of three real samples. This work paves the way for fabricating new highly conductive filaments using a combination of carbon materials with different morphologies and physicochemical properties and their application to produce additively manufactured electrodes with greatly improved electrochemical performance.

Sensitive and selective determination of paracetamol in antipyretic children's syrup with a polyglycine modified glassy carbon electrode.

A sensitive and selective electrochemical sensor for the determination of paracetamol (acetaminophen) is proposed based on a polyglycine-coated glassy carbon electrode. The electrochemical behavior of paracetamol was studied by cyclic voltammetry and differential pulse voltammetry. Under optimal experimental conditions, the peak oxidation current of paracetamol increases linearly in the range of 0.5-75 µM. The limit of detection of paracetamol was 0.03 µM and the limit of quantitation was 0.09 µM. In addition, modified glassy carbon with polyglycine as the sensor was successfully used for the determination of paracetamol in antipyretic children's syrup samples, with a recovery rate of over 95.3%, showing its great application potential in drug analysis.

Polyester resin and graphite flakes: turning conductive ink to a voltammetric sensor for paracetamol sensing.

The development of a disposable electrochemical paper-based analytical device (ePAD) is described using a novel formulation of conductive ink that combines graphite powder, polyester resin, and acetone. As a proof of concept, the proposed sensor was utilized for paracetamol (PAR) sensing. The introduced ink was characterized via morphological, structural, and electrochemical analysis, and the results demonstrated appreciable analytical performance. The proposed ePAD provided linear behavior (R2 = 0.99) in the concentration range between 1 and 60 µmol L-1, a limit of detection of 0.2 µmol L-1, and satisfactory reproducibility (RSD ~ 7.7%, n = 5) applying a potential of + 0.81 V vs Ag at the working electrode. The quantification of PAR was demonstrated in different pharmaceutical formulations. The achieved concentrations revealed good agreement with the labeled values, acceptable accuracy (101% and 106%), and no statistical difference from the data obtained by HPLC at the 95% confidence level. The environmental impact of the new device was assessed using AGREE software, which determined a score of 0.85, indicating that it is eco-friendly. During the pharmacokinetic study of PAR, it was found that the drug has a maximum concentration of 23.58 ± 0.01 µmol L-1, a maximum time of 30 min, and a half-life of 2.15 h. These results are comparable to other studies that utilized HPLC. This suggests that the combination of graphite powder and polyester resin can transform conductive ink into an effective ePAD that can potentially be used in various pharmaceutical applications.

Assessment of selected pharmaceuticals in Riyadh wastewater treatment plants, Saudi Arabia: Mass loadings, seasonal variations, removal efficiency and environmental risk.

Despite increasing interest in pharmaceutical emissions worldwide, studies of environmental contamination with pharmaceuticals arising from wastewater discharges in Saudi Arabia are scarce. Therefore, this study examined occurrence, mass loads and removal efficiency for 15 pharmaceuticals and one metabolite (oxypurinol) from different therapeutic classes in three wastewater treatment plants (WWTPs), in Riyadh city in Saudi Arabia. A total of 144 samples were collected from the influents and effluents between March 2018 and July 2019 and analyzed using Solid Phase Extraction followed by triple quadrupole LC-MS/MS. The average concentrations in the influents and effluents were generally higher than their corresponding concentrations found either in previous Saudi Arabian or global studies. The four most dominant compounds in the influent were acetaminophen, ciprofloxacin, caffeine, and diclofenac, with caffeine and acetaminophen having the highest concentrations ranging between 943 and 2282 µg/L. Metformin and ciprofloxacin were the most frequently detected compounds in the effluents at concentrations as high as 33.2 µg/L. Ciprofloxacin had the highest mass load in the effluents of all three WWTPs, ranging between 0.20 and 20.7 mg/day/1000 inhabitants for different WWTPs. The overall average removal efficiency was estimated high (≥80), with no significant different (p > 0.05) between the treatment technology applied. Acetaminophen and caffeine were almost completely eliminated in all three WWTPs. The samples collected in the cold season generally had higher levels of detected compounds than those from the warm seasons, particularly for NSAID and antibiotic compounds. The estimated environmental risk from pharmaceutical compounds in the studied effluents was mostly low, except for antibiotic compounds. Thus, antibiotics should be considered for future monitoring programmes of the aquatic environment in Saudi Arabia.