كلية الصيدلة الإكلينيكية|College of Clinical Pharmacy

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Evaluation of solvent and temperature effect on green accelerated solvent extraction (ASE) and UHPLC quantification of phenolics in fresh olive fruit (Olea europaea),
(2021) Rizwan Ahmad; Niyaz Ahmad; Ahmed Aljamea; Saad Abuthayn; Mohammed Aqeel
A green ASE (accelerated solvent extraction) with a shorter UHPLC (ultra-high performance liquid chromatography) method was developed for simultaneous determination of phenolics. High extract yield (130آ mg/g) was observed for water at 100آ آ°C in a short time of 19.5آ min using 33.5آ mL solvent whereas, UHPLC showed more phenolics of GA (gallic acid), QT (quercetin), LT (luteolin) in ACE (acetone) and RT (rutin) in EtOH (ethanol) solvent at 60آ آ°C. The binary solvent system of ACE: EtOH (1:1) at 60آ آ°C was optimized as extraction set. UHPLC runtime was 3آ min with retention times of (min); 0.63 (GA), 0.97 (RT), 2.00 (QT) and 2.41 (LT). Average for phenolics (ppm) was, QT (10.91)آ >آ GA (7.33)آ >آ LT (4.10)آ >آ RT (3.90) whereas, Spanish whole green olive (SP2) showed more phenolics (20.72). Individual phenolic was, GA (47.06)آ >آ RT (26.21)آ >آ QT (19.34)آ >آ LT (6.18). Multivariate, K-mean and PCA (principal component analysis) for solvent*extract yield showed significant correlation and temperature showed no significant correlation for phenolics.
Preparation and In Vitro-In Vivo Evaluation of Luteolin Loaded Gastroretentive Microsponge for the Eradication of Helicobacter pylori Infections
(2021) M. S. Jafar, MohammedKhan, Mohd Sajjad AhmadAlshehry, YasirAlrwaili, Nazar RadwanAlzahrani, Yazeed AliImam, Syed SarimAlshehri, Sultan
Combinatorial Regimen of Carbamazepine and Imipramine Exhibits Synergism against Grandmal Epilepsy in Rats: Inhibition of Pro-Inflammatory Cytokines and PI3K/Akt/mTOR Signaling Pathway
(2021) F. H. S. Pottoo, Mohammed; Khan, Firdos Alam; AL Dhamen, Marwa Abdullah; Alsaeed, Walaa Jafar; Gomaa, Mohamed S.; Vatte, Chittibabu; Alomary, Mohammad N.
Epilepsy is a neurodegenerative disorder that causes recurring seizures. Thirty-five percent of patients remain refractory, with a higher prevalence of depression. We investigated the anticonvulsant efficacy of carbamazepine (CBZ; 20 and 50 mg/kg), imipramine (IMI; 10 and 20 mg/kg) alone, and as a low dose combination. This preclinical investigation included dosing of rats for 14 days followed by elicitation of electroshock on the last day of treatment. Along with behavioral monitoring, the rat hippocampus was processed for quantification of mTOR, IL-1β, IL-6 and TNF-α levels. The histopathological analysis of rat hippocampus was performed to ascertain neuroprotection. In vitro studies and in silico studies were also conducted. We found that the low dose combinatorial therapy of CBZ (20 mg/kg) + IMI (10 mg/kg) exhibits synergism (p < 0.001) in abrogation of maximal electroshock (MES) induced convulsions/tonic hind limb extension (THLE), by reducing levels of pro-inflammatory cytokines, and weakening of the PI3K/Akt/mTOR signal. The combination also exhibits cooperative binding at the Akt. As far as neuroprotection is concerned, the said combination increased cell viability by 166.37% compared to Pentylenetetrazol (PTZ) treated HEK-293 cells. Thus, the combination of CBZ (20 mg/kg) + IMI (10 mg/kg) is a fruitful combination therapy to elevate seizure threshold and provide
Thymoquinone Potentiates the Effect of Phenytoin against Electroshock-Induced Convulsions in Rats by Reducing the Hyperactivation of m-TOR Pathway and Neuroinflammation: Evidence from In Vivo, In Vitro and Computational Studies
(2021) F. H. S. Pottoo, Mohammed; Khan, Firdos Alam; Alomar, Fadhel; AL Dhamen, Marwa Abdullah; Alhashim, Abrar Fouad; Alqattan, Hawra Hussain; Gomaa, Mohamed S.; Alomary, Mohammad N.
Epilepsy is a chronic neurodegenerative disease characterized by multiple seizures, hereto 35% of patients remain poor responders. Phenytoin (PHT; 20 and 40 mg/kg) and thymoquinone (THQ; 40 and 80 mg/kg) were given alone and as a low dose combination for 14 days (p.o), prior to challenge with maximal electroshock (MES; 180 mA, 220 V, 0.2 s). Apart from observing convulsions, hippocampal mTOR, IL-1β, IL-6 and TNF-α levels were measured. Hippocampal histomorphological analysis was also conducted. In vitro cell line studies and molecular docking studies were run in parallel. The results revealed the synergistic potential of the novel duo-drug combination regimen: PHT (20 mg/kg) and THQ (40 mg/kg) against MES-induced convulsions. MES amplified signaling through mTOR, and inflated the levels of proinflammatory markers (IL-1β, IL-6 and TNF-α), which was significantly averted (p < 0.001) with the said drug combination. The computational studies revealed that PHT and THQ cooperatively bind the active site on Akt (upstream target of m-TOR) and establish a good network of intermolecular interactions, which indicates the sequential inhibition of PI3K/Akt/m-TOR signaling with the combination. The combination also increased cell viability by 242.81% compared to 85.66% viability from the the toxic control. The results suggest that the PHT and THQ in combination possesses excellent anticonvulsant and neuroprotective effects.
Green accelerated solvent extraction (ASE) with solvent and temperature effect and green UHPLC-DAD analysis of phenolics in pepper fruit (Capsicum annum L.),
(2021) Rizwan Ahmad; Niyaz Ahmad; Sadeq Alkhars; Ali Alkhars; Mohammed Alyousif; Ali Bukhamseen; Saad Abuthayn; Mohammed Aqeel; Ahmed Aljamea
The study presents for the first time, a green and efficient accelerated solvent extraction (ASE) method for phenolic compounds (GA gallic acid, QT quercetin, RT rutin, LT luteolin) with simultaneous determination using a green and effective UHPLC-DAD method. The effect of solvents (ACE acetone, EtOH ethanol, and H2O water) and temperatures (60, 80, 100 °C) Vs extract yield and phenolic recovery was investigated. The scale-up for ASE-UHPLC method was accomplished in 27 food-grade samples of Capsicum annum/pepper fruit (PF). ASE-MD (method development) showed a high extract yield (198.23 mg/g) in water (33 mL) at 100 °C within a time frame of 19.5 min. UHPLC-DAD revealed more yield for GA in ACE whereas, for RT, QT, LT in EtOH at 60 °C. Binary solvent system (ACE: EtOH; 1:1) and 60 °C was optimized the extraction set. The UHPLC-MDMV showed a run time of 5 min with individual retention times of 0.667 (GA), 1.05 (RT), 3.24 (QT), and 3.78 (LT) in the linearity range (1–100 ppm). The average for phenolics (ppm) in 27 PF-food samples was; GA (19.46) > QT (10.19) > LT (4.06) > RT (2.41). SP4 (Spanish green bell pepper) sample showed more amount of total phenolics (32.52 ppm, 25.36 %) whereas, the order for individual phenolic amount (ppm) was; GA (53.39) > QT (13.58) > RT (10.04) > LT (4.62). Multivariate analysis resulted a significant correlation for solvent*temperature with extract yield but with a lack of correlation for phenolics amount. K-mean correlation was positive for solvent Vs phenolic yield (P < 0.05) whereas, extract yield and temperature were less significant for phenolics content. Solvent established a high significant role for extraction and phenolic recovery whereas, temperature was more significant for extract yield rather than phenolic amount.
ICP-MS determination of elemental abundance in traditional medicinal plants commonly used in the Kingdom of Saudi Arabia
(2022) R. S. Ahmad, H.; Sara Algarni; Rand Osama; Alghamdi, M.; Njoud Hamid; Rizwan Ahmad; Algarni, S.; Mostafa, A.; Abdulmalik Alqarni; Aldholmi, M.; Riaz, M.
Medicinal plants are widely used in the Kingdom of Saudi Arabia to treat various ailments in the form of folk medicine. Forty four such medicinal plant samples were collected from local markets and evaluated for the presence of 14 elements (Mn, Cr, Co, Ni, Cu, Mo, Al, Pb, Ba, Zn, Ag, Hg, Bi, Cd). Microwave-assisted digestion with inductively coupled plasma-mass spectrometry (ICP-MS) was applied to determine the elemental composition in these medicinal plants. Widespread occurrence of these elements was observed in all plant samples, except for Bi and Co where the lowest mean values of 0.03 ± 0.04 and 0.03 ± 0.15 were observed, respectively. The descending order for mean (μg/g) elemental occurrence observed was as follows: Ba > Al > Zn > Ni > Mn > Ba > Hg > Mo > Cu > Cr > Ag > Cd > Co > Bi, whereas the range for these elements in the 44-medicinal plants was as follows: Pb > Al > Zn > Ni > Mn > Cu > Mo > Ag > Ba > Hg > Co > Cd > Cr > Bi. Pb, Hg and Cd were found beyond the maximum limits in these medicinal plants, while the remaining elements were found well within the range of maximum limits. A number of medicinal plants showed high amounts of these elements. Some plants contained more than one element, such as Foeniculum vulgare Mill (Pb, Hg, Cd), Ricinus communis (Pb, Cd), Vigna radiata (Pb, Cd) and Sesamum indicum (Pb, Hg). The data matrix was validated through the statistical tools of principal component analysis (X(2) = 160.44, P = .00), Pearson's correlation (P = .01 and 0.05), and K-mean cluster analysis (F = 104.55, P = .00). The findings of the study provide baseline data for the comparative analysis of these medicinal plants, which may help select safe medicinal plants in terms of consumer-based use and its utilisation for the treatment of various ailments.
Vortex-assisted dispersive liquid–liquid microextraction using thymol based natural deep eutectic solvent for trace analysis of sulfonamides in water samples: Assessment of the greenness profile using AGREE metric, GAPI and analytical eco-scale
(2022) Sahar Tawfiq Taher Alsaba; Amal Abdullah Saleh almoslem; Alqarni, Abdulmalik M.; Alghamdi, Meshal; Alsultan, Semat; Heba Shaaban Mohamed; Alsaba, Sahar; AlMoslem, Amal; Alshehry, Yasir; Ahmad, Rizwan
Applying the concepts of green analytical chemistry (GAC) across the whole method development is gaining more interest with the aim of using eco-friendly solvents and minimizing waste generation. Therefore, replacing the conventional methods with benign alternatives has been the aim of many researchers and practitioners worldwide. Natural deep eutectic solvents (NDESs) can be considered as a green alternative to the toxic organic solvents. In this work, a thymol based NDES was utilized for the first time in the extraction and trace analysis of four different sulfonamides (Sulfapyridine, sulfamethazine, sulfamethoxazole and Sulfaphenazole) in different water samples using dispersive liquid–liquid microextraction (DLLME). Two different groups of hydrophobic NDESs were prepared and tested as microextraction solvents, using the natural monoterpenoids (menthol and thymol) in combination with different acids and an alcohol. The results revealed that thymol/acetic acid DES had the best extraction recovery. Dispersion of the extracting solvents was achieved via vortex mixing. All DLLME parameters were optimized. The optimized method showed low detection limits (0.78 – 3.42 ng mL−1). A good linearity (5–5000 ng mL−1) with excellent determination coefficients (r2 ≥ 0.9991) was obtained. Accuracy and precision showed good results with % recovery in the range of 81.3–105.2 % and %RSD ranging from 1.3 to 7.9. The proposed method was successfully applied for the trace analysis of the target analytes in different water samples. Finally, the greenness profile was assessed by Analytical Eco-scale, Green Analytical Procedure Index (GAPI) and AGREE metric and comparison showed the superiority of the proposed method over other published methods. In conclusion, the reported method can be considered as a valid eco-friendly alternative for the classical and conventional hydrophobic DES-based DLLME methods for the routine analysis of sulfonamides in different water samples.
A novel green extraction and analysis technique for the comprehensive characterization of mangiferin in different parts of the fresh mango fruit (Mangifera indica)
(2022) Saeed Abdullah Aldossary; Salem Mohammed Bubshait; Aljawharah, Alqathama; Alaa, Aldarwish; Asma, Abuhassan; Leena, Alateeq; Rizwan Ahmad; Mohammed jaber G Aldholmi; Saeed, Aldossary
The study reports a novel, green, and effective ASE (accelerated solvent extraction) technique with a green, fast, and sensitive method of UPLC-MS/MS for a comprehensive characterization of whole mango fruit (epi-, endo-, Mesocarp, seed) under solvent, temperature, and origin effect in order to determine the inter- and intra-variation of MG(Mangiferin)-amount in fresh mango fruit. The ASE-MD (method development) showed the highest extract yield and more MG-amount in H2O at 80 °C (mesocarp fruit part). For MG-quantification, a fast and sensitive UPLC-MS/MS method (RT = 0.31/runtime = 1 min; m/z 421.10 → 81.00 amu) was developed. The UPLC-MS/MS-MV validated the method with high accuracy, precision, and r2 = 0.998. The intra-variation for MG was: mesocarp > endocarp > epicarp > seed. The inter-variation (MG-amount (mg/10g) in 12-mango cultivars) based on the sum of MG-amount/12-mango fruits parts: mesocarp (12.42)> epicarp (10.92)> endocarp (10.47)> seed (8.70) whereas, based on the largest MG-amount/individual mango fruit it was: mesocarp (5/12 fruits)> endocarp (4/12 fruits)> epicarp (3/12 fruits)> seed (0/12). The statistical models for PCA, K-mean cluster, and Pearson's analysis revealed significant correlation (P ≤ 0.005) for origin*solvent*temperature Vs MG-amount with a nonsignificant correlation for origin*MG-amount Vs extract yield. The ASE-UPLC-MS/MS comprehensively characterized inter-, and intra-variation of MG in different parts of mango fruit.
Assessment of self-medication practice and the potential to use a mobile app to ensure safe and effective self-medication among the public in Saudi Arabia
(2022) Alsaad, Hassan A.; Almahdi, Jenan Saleh; Mohammad Ashraful Islam; Alomar, Fadhel Ahmed; Islam, Md Ashraful
Background Self-medication (SM) plays an essential role in maintaining a good quality of life for individuals. Previous studies suggested that efforts are still needed to ensure the safe practice of SM. The advances in technology and the internet have granted the availability of abundant and easily accessed medication information. However, identifying the reliability of information could be a challenge for the public. This study aimed to investigate the attitude toward SM, determinants of SM, and knowledge about medication in Saudi Arabia. Also, this study aimed to assess the willingness to use a mobile app that would be specifically designed to guide the practice of SM. Methods A cross-sectional study was conducted in a form of an online survey among the public in Saudi Arabia. QuestionPro® platform was utilized to collect data from respondents for two months. Statistical analysis was performed using IBM® SPSS® statistics version 26. Results A total of 1226 individuals completed the questionnaire. The prevalence of SM practice was 59%. The most frequent reason for not practicing SM was the concern about the drug safety issues (38%). Significant statistical associations were identified between SM and several demographic variables, e.g., age, gender, education, health insurance, and having a chronic illness. Most respondents (82.7%) were aware of the necessity of improving SM practice. Knowledge about different aspects of SM (e.g., proper drug selection and administration) was evaluated based on the consumer’s perspective. Our data showed that overall knowledge about SM was limited for many consumers. The assessment of the participant’s willingness to use a SM app indicated that 47.6% were interested in using such app. This willingness was significantly associated with the consumer’s attitude toward SM and being a chronically ill patient. Conclusion
Thymoquinone: Review of Its Potential in the Treatment of Neurological Diseases
(2022) Mahdi Mohammed Muslim Aleid; Alammar, Ali; Alsinan, Rida; Faheem Hyder Pottoo; Abdullah mohammed Ibrahim; Muruj Ahmed Alshehri; Mishra, Supriya; Alhajri, Noora
Simultaneous determination of bisphenol A and its analogues in foodstuff using UPLC-MS/MS and assessment of their health risk in adult population
(2022) S. A. Heba, Mostafa; Abdulmalik, M. Alqarni; Yasmeen, Almohamed; Duaa, Abualrahi; Dania, Hussein; Abdulmalik Alqarni; Meshal Alghamdi
Replacing bisphenol A with its analogues may represent a risk to human health because of their potential synergic effects. In this study, a fast, sensitive and reliable UPLC-MS/MS method for the identification and quantification of bisphenol A, bisphenol F, bisphenol S, D8 and pergafast in foodstuff was developed and validated. Sample preparation and clean up were carried out using ultrasonic extraction followed by solid-phase extraction on Oasis HLB cartridges. The developed method was successfully applied for simultaneous determination of the target analytes in 140 food samples from various categories (including: vegetables, dairy products, seafood products, condiments, beverages, oils & fats and others). The recovery ranged from 80.3% to 103.8% with relative standard deviations not higher than 11.5%. Limits of detection were within the range of 0.003–0.015 μg kg−1 under the optimized conditions. Bisphenol A was found in the majority of food samples (83%) with the highest concentration of 110 µg kg−1. Canned food contained higher concentrations of total bisphenols (23.8 µg kg−1) compared to food samples packed in plastic containers (7.68 µg kg−1), paper (3.53 µg kg−1) or glass (1.14 µg kg−1). The estimated daily intake for the detected bisphenols was also calculated (286.7 and 307.8 ng kg−1 BW day−1) for male and female adults, respectively. The dietary exposure to total bisphenols through foodstuffs investigated in this study were found to be higher than the recently updated tolerable daily intake value of BPA (0.04 ng kg−1 BW day−1). Also, the calculated hazard index was found to be higher than 1, indicating that the exposure to the detected bisphenols is more likely to cause risk to consumers through the dietary intake. To the best of our knowledge, this is the first report estimating the health risk associated with dietary exposure to bisphenol A and its analogues in Saudi Arabia.
Efficacy of Core Training in Swimming Performance and Neuromuscular Parameters of Young Swimmers: A Randomised Control Trial
(2022) Ahmad Khiyami; Nuhmani, Shibili; Joseph, Royes; Turki Saeed Abualait; Muaidi, Qassim
Background: This study aimed to investigate the efficacy of core training in the swimming performance and neuromuscular properties of young swimmers. Methods: Eighteen healthy male swimmers (age: 13 ± 2 years, height: 159.6 ± 14.5 cm, weight: 48.7 ± 12.4 kg) were recruited from the Public Authority for Sports swimming pool in Dammam and randomly assigned to the experimental and control groups. The experimental group performed a six-week core-training program consisting of seven exercises (three times/week) with regular swimming training. The control group maintained its regular training. Swimming performance and neuromuscular parameters were measured pre- and post-interventions. Results: The experimental group benefitted from the intervention in terms of the 50 m swim time (−1.4 s; 95% confidence interval −2.4 to −0.5) compared with the control group. The experimental group also showed improved swimming velocity (+0.1 m.s−1), stroke rate (−2.8 cycle.min−1), stroke length (+0.2 m.cycle−1), stroke index (+0.4 m2·s−1), total strokes (−2.9 strokes), and contraction time for erector spinae (ES; −1.5 ms), latissimus dorsi (LD; −7 ms), and external obliques (EO; −1.9 ms). Maximal displacement ES (DM-ES) (+3.3 mm), LD (0.5 mm), and EO (+2.2 mm) were compared with the baseline values for the experimental group, and TC-ES (5.8 ms), LD (3.7 ms), EO (2.5 ms), DM-ES (0.2 mm), LD (−4.1 mm), and EO (−1.0 mm) were compared with the baseline values for the control group. The intergroup comparison was statistically significant (p < 0.05; DM-ES p > 0.05). Conclusion: The results indicate that a six-week core-training program with regular swimming training improved the neuromuscular properties and the 50 m freestyle swim performance of the experimental group compared with the control group.
Beta blockers may be protective in COVID-19; findings of a study to develop an interpretable machine learning model to assess COVID-19 disease severity in light of clinical findings, medication history, and patient comorbidities
(2023) Manar Alghamdi; Sarah Almustafa; Mona Alshamery; Rand Al-abdulmohsin; Laila Al Rabia; Al-abdulmohsin, Rand; Nawal Alsheikh; Al Nass, Fatimah; Alghamdi, Manar; Sawsan Kurdi; Mohammad Ashraful Islam; Kurdi, Sawsan; Zainab Aljamea; Hussein, Dania
The coronavirus disease 2019 (COVID-19) has overwhelmed healthcare systems and continues to pose a significant threat worldwide. Predicting disease severity would enhance treatment provision and resource allocation. Although multiple studies were conducted to assess COVID-19's severity using machine learning (ML) models, few studies focus on patient medication history and comorbidities. In this study, ML algorithms were trained using a comprehensive dataset comprising medication history, comorbidities, and clinical findings. Patient data was gathered from King Fahad University Hospital (KFUH) in Saudi Arabia (IRB#: 2021-05-480). The dataset comprised 622 positive COVID-19 with 49 features. Three experiments were conducted to train four ML algorithms, including random forest (RF), gradient boosting machine (GMB), extreme gradient boost (XGBoost), and extra trees (ET). Findings revealed that GBM outperformed other models with 96.30% accuracy, 95.80% precision, 97.64% recall, and 96.69% F-score, with 23 features. Moreover, the permutation feature importance technique suggested that the five most influential features for forecasting disease severity were “CRP level”, “CO2 level”, “SrCr”, “Tocilizumab”, and “Age”. In addition, the shapley additive explanation (SHAP) recommended that the “D-Dimer level”, “CrCl”, and “Hypertension” were also influential. The development of an effective GBM model has the potential to aid medical specialists in the assessment of disease severity. While several models take into account patient presentation and laboratory findings, this study is unique in its scope, considering a far more comprehensive patient profile. The developed model was able to accurately predict features that have been clinically shown to correlate with disease severity. Of interest the model was able to identify a pattern of association between the use of certain medications such and disease severity. We report that the use of beta blockers may be associated with reduced severity, whereas the use of immune modulating drugs namely tocilizumab appeared to be associated with poor disease outcomes in this patient population.
Development and optimization of natural deep eutectic solvent-based dispersive liquid–liquid microextraction coupled with UPLC-UV for simultaneous determination of parabens in personal care products: evaluation of the eco-friendliness level of the developed method
(2023) Atheer Aseeri; Mostafa, Ahmed; Nujud Bakhashwain; Gomaa, Mohamed S.; Abdulmalik M. AlQarni; Ahmed Mohamed Mostafa; Bakhashwain, Nujud; Aseeri, Atheer; Alqarni, Abdulaziz; Alamri, Abdulgani A.; Alrofaidi, Mohammad A.
Dispersive liquid–liquid microextraction (DLLME) combined with ultra-high performance liquid chromatography-diode array detector (UHPLC-DAD) method has been developed and validated for the determination of parabens in personal care products. In this study, a natural deep eutectic solvent (NADES) composed of menthol and formic acid at a molar ratio of 1 : 2 was prepared and used as an extraction solvent. The influencing variables on the extraction efficiency such as extraction solvent type and volume, composition of NADES, salt addition, vortex and centrifugation time were investigated. The proposed method exhibited good linearity with determination coefficients of ≥0.9992. The relative recoveries for the studied analytes ranged from 82.19 to 102.45%. Limits of detection and limits of quantification were in the range of 0.17–0.33 ng mL−1 and 0.51–0.99 ng mL−1, respectively. To evaluate the applicability of the developed method, it was successfully applied to determine four parabens in personal care products. Additionally, the eco-friendliness level of the presented method was evaluated using Eco-Scale Assessment, Green Analytical Procedure Index and Analytical GREEnness metric. The developed method is simple, environmentally friendly and cost effective and it could be employed for determination of parabens in personal care products without harming the environment.
Development and optimization of natural deep eutectic solvent-based dispersive liquid–liquid microextraction coupled with UPLC-UV for simultaneous determination of parabens in personal care products: evaluation of the eco-friendliness level of the developed method
(2023) Alqarni, Abdulmalik M.; Mostafa, Ahmed; Nujud Bakhashwain; Batool Hasheeshi; Albashrayi, Danyah; Hasheeshi, Batool; Heba shaaban Mohamed; Aseeri, Atheer; Alqarni, Abdulaziz; Alamri, Abdulgani A.; Alrofaidi, Mohammad A.
Dispersive liquid–liquid microextraction (DLLME) combined with ultra-high performance liquid chromatography-diode array detector (UHPLC-DAD) method has been developed and validated for the determination of parabens in personal care products. In this study, a natural deep eutectic solvent (NADES) composed of menthol and formic acid at a molar ratio of 1 : 2 was prepared and used as an extraction solvent. The influencing variables on the extraction efficiency such as extraction solvent type and volume, composition of NADES, salt addition, vortex and centrifugation time were investigated. The proposed method exhibited good linearity with determination coefficients of ≥0.9992. The relative recoveries for the studied analytes ranged from 82.19 to 102.45%. Limits of detection and limits of quantification were in the range of 0.17–0.33 ng mL−1 and 0.51–0.99 ng mL−1, respectively. To evaluate the applicability of the developed method, it was successfully applied to determine four parabens in personal care products. Additionally, the eco-friendliness level of the presented method was evaluated using Eco-Scale Assessment, Green Analytical Procedure Index and Analytical GREEnness metric. The developed method is simple, environmentally friendly and cost effective and it could be employed for determination of parabens in personal care products without harming the environment.
Dispersive liquid-liquid microextraction utilizing menthol-based deep eutectic solvent for simultaneous determination of sulfonamides residues in powdered milk-based infant formulas
(2023) Shahad Osama AlKahlah; Mostafa, Ahmed; Ruya Alsultan; Zahrra Dheya AlJarrash; Weaam Mustafa Alzawad; Aljarrash, Zahra; Al-Zawad, Weaam; Ahmed Mohamed Mostafa; Amir, Mohd
An eco-friendly, fast, sensitive dispersive liquid–liquid microextraction (DLLME) method followed by UPLC-MS/MS was developed and validated for multi-residue determination of sulfonamides in milk-based infant and young children formulas. In this study, a natural deep eutectic solvent was synthesized using menthol and octanoic acid at a molar ratio of 1:2 for the extraction of seven sulfonamides in infant formulas. Different extraction parameters including volume of deep eutectic solvent, vortex time, centrifugation time, sample volume and pH were investigated and optimized. Under the optimum conditions, determination coefficients of ≥ 0.9993 were obtained for all studied analytes. The limits of detection ranged from 0.5 to 1.5 µg Kg−1. The extraction recoveries were in the range of 82.6–100.1% with RSDs %≤ 7.5. To investigate the applicability of the proposed method, it was applied to determination of the studied sulfonamides in thirty milk-based infant formulas of different brands. The environmental impact of the presented method was evaluated using three assessment tools namely: Eco-Scale Assessment (ESA), Green Analytical Procedure Index (GAPI) and Analytical GREEnness metric (AGREE). The characteristic performance of the developed DLLME-UPLC-MS/MS method was also compared with other reported methods.
Multi-class determination of pharmaceuticals as emerging contaminants in wastewater from Eastern Province, Saudi Arabia using eco-friendly SPE-UHPLC-MS/MS: Occurrence, removal and environmental risk assessment
(2023) Mohammed Abdulhadi M Alsulaiman; Fatimah Lutfi H Alsaif; Alqarni, Abdulmalik; Al-Ansari, Raneem; Abdulmalik Mohammed H Alqarni; Al-Sultan, Fatima; Alsulaiman, Mohammed; Alsaif, Fatimah; Aga, Omer
Occurrence of pharmaceuticals in wastewater, which might be released to different water environments causing contamination might lead to health hazards. Therefore, sensitive, selective and reliable analytical methods are required to monitor pharmaceuticals in such complex environmental matrix. In this work, an eco-friendly, sensitive, robust and selective ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) method was developed to simultaneously identify and quantify multiple classes of pharmaceuticals in influent and effluent wastewater samples in Eastern Province, Saudi Arabia using solid phase extraction (SPE) for sample preparation. The extraction conditions were optimized to achieve the best extraction efficiencies and achieved recoveries of 70.4 – 112.2% and 74.0 – 107.8% in influent (IWW) and effluent wastewater (EWW) samples, respectively. The optimized method had satisfactory precision represented as %RSD lower than 13.04%. Limits of detection were 0.06 – 16.0 and 0.07 – 13.23 ng L-1 for IWW and EWW, respectively. The developed method was successfully employed for the analysis of 32 pharmaceuticals in wastewater. The greenness profile was assessed using two assessment tools; Analytical Eco-scale and AGREE metric. Caffeine and Ciprofloxacin were the most frequent and highest concentration in influent wastewater with concentration range 23,600 – 37,602 ng L-1 and 1,684 –3,585 ng L-1, respectively. Average effluent concentrations range was from below method quantification limit to 1,241 ng L-1 (ciprofloxacin). Removal efficiency ranged from - 3.1% (trimethoprim) to 99% (caffeine). Environmental risk assessment was calculated using risk quotient approach for each individual analyte and for the mixture. The results revealed 4 and 6 compounds with high and medium risk, respectively. This work provides new insights into the occurrence, removal and ecotoxicological risk of pharmaceuticals from wastewater in Eastern Province, Saudi Arabia. It emphasizes the importance of monitoring these compounds as an input for future mitigation actions.
Biological Screening of Glycyrrhiza glabra L. from Different Origins for Antidiabetic and Anticancer Activity
(2023) Abdulmalik Eissa Mossa Ayashy; Alqathama, Aljawharah; Aldholmi, Mohammed; Rizwan Ahmad; Mohammed Jaber G Aldholmi; Aljishi, Fatema; Althomali, Ebtihal; Alamer, Muntathir Ali; Alsulaiman, Mohammed; Ayashy, Abdulmalik; Alshowaiki, Mohsen
Background: Geographical variation may affect the phytochemistry as well as the biological activities of Glycyrrhiza glabra (licorice) root. Herein, a series of biological activities were performed to evaluate the impact of geographical origin on the biological potential of eight different licorice samples. Methodology: Cell culture studies were performed for cytotoxicity (MCF7, HCT116, HepG2, and MRC5), glucose uptake assay (HepG2), and glutathione peroxidase activity (HepG2), whereas α-amylase inhibition activity was tested for antidiabetic potential. Results: The Indian sample was observed to be more cytotoxic against MCF7 (22%) and HCT116 (43%) with an IC50 value of 56.10 (±2.38) μg/mL against the MCF7 cell line. The glucose uptake was seen with a mean value of 96 (±2.82) and a range of 92–101%. For glutathione peroxidase activity (GPx), the Syrian (0.31 ± 0.11) and Pakistani samples (0.21 ± 0.08) revealed a significant activity, whereas the Palestinian (70 ± 0.09) and Indian samples (68±0.06) effectively inhibited the α-amylase activity, with the lowest IC50 value (67.11 ± 0.97) μg/mL for the Palestinian sample. The statistical models of PCA (principal component analysis) and K-mean cluster analysis were performed to correlate the geographical origin, extract yield, and biological activities for the eight licorice samples of different origins. Conclusion: The licorice samples exhibited significant cytotoxic, GPx, and α-amylase inhibitory activity. The samples with higher extract yield showed more potential in these biological activities.

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