Displaying publications 1 - 20 of 42 in total

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  1. Agatonovic-Kustrin S, Wong S, Dolzhenko AV, Gegechkori V, Morton DW
    J Pharm Biomed Anal, 2024 Feb 15;239:115912.
    PMID: 38128161 DOI: 10.1016/j.jpba.2023.115912
    Olive trees are one of the most widely cultivated fruit trees in the world. The chemical compositions and biological activities of olive tree fruit and leaves have been extensively researched for their nutritional and health-promoting properties. In contrast, limited data have been reported on olive flowers. The present study aimed to analyse bioactive compounds in olive flower extracts and the effect of fermentation-assisted extraction on phenolic content and antioxidant activity. High-performance thin-layer chromatography (HPTLC) hyphenated with the bioassay-guided detection and spectroscopic identification of bioactive compounds was used for the analysis. Enzymatic and bacterial in situ bioassays were used to detect COX-1 enzyme inhibition and antibacterial activity. Multiple zones of antibacterial activity and one zone of COX-1 inhibition were detected in both, non-fermented and fermented, extracts. A newly developed HPTLC-based experimental protocol was used to measure the high-maximal inhibitory concentrations (IC50) for the assessment of the relative potency of the extracts in inhibiting COX-1 enzyme and antibacterial activity. Strong antibacterial activities detected in zones 4 and 7 were significantly higher in comparison to ampicillin, as confirmed by low IC50 values (IC50 = 57-58 µg in zone 4 and IC50 = 157-167 µg in zone 7) compared to the ampicillin IC50 value (IC50 = 495 µg). The COX-1 inhibition by the extract (IC50 = 76-98 µg) was also strong compared to that of salicylic acid (IC50 = 557 µg). By comparing the locations of the bands to coeluted standards, compounds from detected bioactive bands were tentatively identified. The eluates from bioactive HPTLC zones were further analysed by FTIR NMR, and LC-MS spectroscopy. Multiple zones of antibacterial activity were associated with the presence of triterpenoid acids, while COX-1 inhibition was related to the presence of long-chain fatty acids.
  2. Roslan A, Said DS, Sulaiman N, Mohd Ghani KA, Nurdin A
    J Pharm Biomed Anal, 2023 Nov 30;236:115729.
    PMID: 37778199 DOI: 10.1016/j.jpba.2023.115729
    Studies reveal that alterations in membrane protein (MP) patterns are associated with underlying drug resistance to chemotherapy. Therefore, the tryptic-digested MPs from the bladder cancer cell line were subjected to global proteomics using LC-MS/MS to identify the highly expressed potential MPs in bladder cancer cells. Our findings revealed the identification of MP biomarkers, CD147, and caveolin-1. Immunocytochemistry analysis confirmed the presence of CD147 on the cell membrane, while caveolin-1 showed positive signals without apparent staining on the membrane, suggesting its existence in multiple locations. Western blot analysis confirmed the higher expression of CD147 in non-invasive (RT 112) and metastatic (UM-UC-13) bladder cancer cells compared to invasive bladder cancer cells (5637 and J82), suggesting its potential as an MP biomarker for both of the former subtypes. The identified MPs could be used as drug therapy targets aimed at improving drug sensitivity and enhancing treatment outcomes in bladder cancer patients. SIGNIFICANCE: Identification of the membrane proteins associated with bladder cancer recurrence is crucial to understanding the mechanisms underlying the drug resistance to chemotherapy.
  3. Agatonovic-Kustrin S, Wong S, Dolzhenko AV, Gegechkori V, Ku H, Tan WK, et al.
    J Pharm Biomed Anal, 2023 Apr 01;227:115308.
    PMID: 36827737 DOI: 10.1016/j.jpba.2023.115308
    Extracts of two Salvia species, Salvia apiana (white sage) and Salvia officinalis (common sage) were screened for phytoconstituents with the ability to act as antidiabetic, cognitive enhancing, or antimicrobial agents, by hyphenation of high-performance thin-layer chromatography with enzymatic and microbial effect directed assays. Two bioactive zones with α-amylase inhibition (zone 1 and zone 2), 3 zones for acetylcholinesterase inhibition (zones 3, 4 and 5), and two zones for antimicrobial activity (zones 4 and 5) were detected. The compounds from the five bioactive zones were initially identified by coelution with standards and comparing the RF values of standards to the bioautograms. Identity was confirmed with ATR-FTIR spectra of the isolated compounds from the bioactive zones. A significantly higher α-amylase and acetylcholinesterase inhibition of S. apiana leaf extract was associated with a higher flavonoid and diterpenoid content. Fermented S. officinalis extract exhibited a significantly higher ability to inhibit α-amylase compared to other non-fermented extracts from this species, due to increased extraction of flavonoids. The ATR-FTIR spectra of 2 zones with α-amylase inhibition, indicated that flavonoids and phenolic acids were responsible for α-amylase inhibition. Multiple zones of acetylcholinesterase inhibition were related to the presence of phenolic abietane diterpenoids and triterpenoid acids. The presence of abietane diterpenoids and triterpenoid acids was also found responsible for the mild antimicrobial activity. Flash chromatography was used to isolate sufficient amounts of bioactive compounds for further characterisation via NMR and MS spectroscopy. Five compounds were assigned to the zones where bioactivity was observed: cirsimaritin (zone 1), a caffeic acid polymer (zone 2), 16-hydroxyrosmanol (zone 3), 16-hydroxycarnosic acid (zone 4), oleanolic and ursolic acids (zone 5).
  4. da Silva-Junio AG, Frias IAM, Lima-Neto RG, Migliolo L, E Silva PS, Oliveira MDL, et al.
    J Pharm Biomed Anal, 2022 Jul 15;216:114788.
    PMID: 35525110 DOI: 10.1016/j.jpba.2022.114788
    Bacterial and fungal infections are challenging due to their low susceptibility and resistance to antimicrobial drugs. For this reason, antimicrobial peptides (AMP) emerge as excellent alternatives to overcome these problems. At the same time, their active insertion into the cell wall of microorganisms can be availed for biorecognition applications in biosensing platforms. Temporin-PTA (T-PTA) is an AMP found in the skin secretions of the Malaysian fire frog Hylarana picturata, which presents antibacterial activity against MRSA, Escherichia coli, and Bacillus subtilis. In this work, T-PTA was explored as an innovative sensing layer aiming for the electrochemical differentiation of Klebsiella pneumoniae, Acinetobacter baumannii, Bacillus subtilis, Enterococcus faecalis, Candida albicans, and C. tropicalis based on the structural differences of their membranes. The biosensor was analyzed through electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). In this approach, the different structural features of each microorganism resulted in different adherence degrees and, therefore, different electrochemical responses. The transducing layer was fabricated by the self-assembling of a 4-mercaptobenzoic acid (MBA) monolayer and gold-capped magnetic nanoparticles (Fe3O4@Au) implemented to improve the electrical signal of the biointeraction. We found that each interaction, expressed in variations of electron transfer resistance and anodic peak current, demonstrated a singular response from which the platform can discriminate all different microorganisms. We found expressive sensitivity towards Gram-negative species, especially K. pneumoniae. A detection limit of 101 CFU.mL-1 and a linear range of 101 to 105 CFU.mL-1 were obtained. The T-PTA biosensor platform is a promising and effective tool for microbial identification.
  5. Kamal MSA, Mediani A, Kasim N, Ismail NH, Satar NA, Azis NA, et al.
    J Pharm Biomed Anal, 2022 Feb 20;210:114579.
    PMID: 35016031 DOI: 10.1016/j.jpba.2021.114579
    Ficus deltoidea var angustifolia (FD-A) reduces blood pressure in spontaneously hypertensive rats (SHR) but the mechanism remains unknown. Changes in urine metabolites following FD-A treatment in SHR were, therefore, examined to identify the mechanism of its antihypertensive action. Male SHR were given either FD-A (1000 mg kg-1 day-1) or losartan (10 mg kg-1 day-1) or 0.5 mL of ethanolic-water (control) daily for 4 weeks. Systolic blood pressure (SBP) was measured every week and urine spectra data acquisition, on urine collected after four weeks of treatment, were compared using multivariate data analysis. SBP in FD-A and losartan treated rats was significantly lower than that in the controls after four weeks of treatment. Urine spectra analysis revealed 24 potential biomarkers with variable importance projections (VIP) above 0.5. These included creatine, hippurate, benzoate, trimethylamine N-oxide, taurine, dimethylamine, homocysteine, allantoin, methylamine, n-phenylacetylglycine, guanidinoacetate, creatinine, lactate, glucarate, kynurenine, ethanolamine, betaine, 3-hydroxybutyrate, glycine, lysine, glutamine, 2-hydroxyphenylacetate, 3-indoxylsulfate and sarcosine. From the profile of these metabolites, it seems that FD-A affects urinary levels of metabolites like taurine, hypotaurine, glycine, serine, threonine, alanine, aspartate and glutamine. Alterations in these and the pathways involved in their metabolism might underlie the molecular mechanism of its antihypertensive action.
  6. Muthudoss P, Kumar S, Ann EYC, Young KJ, Chi RLR, Allada R, et al.
    J Pharm Biomed Anal, 2022 Feb 20;210:114581.
    PMID: 35026592 DOI: 10.1016/j.jpba.2022.114581
    Particle size distribution (PSD), spatial location and particle cluster size of ingredients, polymorphism, compositional distribution of a pharmaceutical product are few of the most important attributes in establishing the drug release-controlling microstructural and solid state properties that would be used to (re)design or reproduce similar products. There are numerous solid-state techniques available for PSD analysis. Laser diffraction (LD) is mostly used to study PSD of raw materials. However, a constraint of LD is the interference between the active pharmaceutical ingredients (API) and excipients, where it is very challenging to measure API size in a tablet. X-ray powder diffraction (XRPD) is widely employed in establishing the polymorphism of API and excipients. This research examined a commercial osmotic tablet in terms of extracting solid state properties of API and functional excipient by Raman Imaging. Establishing repeatability, reproducibility, and sample representativeness when the samples are non-uniform and inhomogeneous necessitates multiple measurements. In such scenarios, when employing imaging-based techniques, it can be time-consuming and tedious. Advanced statistical methodologies are used to overcome these disadvantages and expedite the characterization process. Overall, this study demonstrates that Raman imaging can be employed as a non-invasive and effective offline method for assessing the solid-state characteristics of API and functional excipients in complex dosage forms like osmotic tablets.
  7. Saisahas K, Soleh A, Promsuwan K, Phonchai A, Mohamed Sadiq NS, Teoh WK, et al.
    J Pharm Biomed Anal, 2021 Feb 08;198:113958.
    PMID: 33662759 DOI: 10.1016/j.jpba.2021.113958
    A portable electrochemical sensor was developed to determine xylazine in spiked beverages by adsorptive stripping voltammetry (AdSV). The sensor was based on a graphene nanoplatelets-modified screen-printed carbon electrode (GNPs/SPCE). The electrochemical behavior of xylazine at the GNPs/SPCE was an adsorption-controlled irreversible oxidation reaction. The loading of graphene nanoplatelets (GNPs) on the modified SPCE, electrolyte pH, and AdSV accumulation potential and time were optimized. Under optimal conditions, the GNPs/SPCE provided high sensitivity, linear ranges of 0.4-6.0 mg L-1 (r = 0.997) and 6.0-80.0 mg L-1 (r = 0.998) with a detection limit of 0.1 mg L-1 and a quantitation limit of 0.4 mg L-1. Repeatability was good. The accuracy of the proposed sensor was investigated by spiking six beverage samples at 1.0, 5.0, and 10.0 mg L-1. The recoveries from this method ranged from 80.8 ± 0.2-108.1 ± 0.3 %, indicating the good accuracy of the developed sensor. This portable electrochemical sensor can be used to screen for xylazine in beverage samples as evidence in cases of sexual assault or robbery.
  8. Loh GOK, Wong EYL, Tan YTF, Wee HC, Ng RS, Lee CY, et al.
    J Pharm Biomed Anal, 2021 Feb 05;194:113758.
    PMID: 33248861 DOI: 10.1016/j.jpba.2020.113758
    A simple, rapid, sensitive, and reproducible LC-MS/MS method was developed for simultaneous quantification of flavoxate and 3-methyl-flavone-8-carboxylic (MFCA) in human plasma, using diphenhydramine HCl as internal standard (IS). The chromatographic separation was achieved using Agilent Poroshell 120 EC-C18 - Fast LC column (100 × 2.1mmID, 2.7 μm) fitted with UHPLC Guard Poroshell 120 EC-C18 (5 × 2.1 mmID, 2.7 μm). The mobile phase consisted of 0.1 % v/v formic acid and acetonitrile (30:70, v/v) run at a flow rate of 0.40 mL/min. The standard calibration curve was linear over the concentration range of 2.00 - 2,000.31 ng/mL and 240.00 - 24,000.04 ng/mL for flavoxate and MFCA. For flavoxate and MFCA, the within-run precision was 0.81-6.67 % and 1.68-4.37 %, while accuracy was 100.21-108.25 % and 103.99-110.28 %. The between-run precision was 2.01-9.14 % and 2.31-11.11 %, and accuracy was 96.09-103.33 % and 102.37-109.52 %. The extended run precision was 7.78-11.04 % and 2.22-3.33 %, while accuracy was 100.72-101.88 % and 102.34-105.60 %. Flavoxate and MFCA in plasma were stable 4 h at bench top (short term), 24 h in autosampler and instrumentation room (post-preparative), after 7 freeze-thaw cycles, and 89 days in the freezer. Both analytes and IS stock solutions were stable for 31 days when kept at room temperature (25 ± 4 °C) and refrigerated (2-8 °C). The validated method was successfully applied to a bioequivalence study of two flavoxate formulations involving 24 healthy volunteers.
  9. Lim SM, Agatonovic-Kustrin S, Lim FT, Ramasamy K
    J Pharm Biomed Anal, 2021 Jan 30;193:113702.
    PMID: 33160220 DOI: 10.1016/j.jpba.2020.113702
    Bioactive compounds from endophytic fungi exhibit diverse biological activities which include anticancer effect. Capitalising on the abundance of unexplored endophytes that reside within marine plants, this study assessed the anticancer potential of ethyl acetate endophytic fungal extracts (i.e. MBFT Tip 2.1, MBL 1.2, MBS 3.2, MKS 3 and MKS 3.1) derived from leaves, stem and fruits of marine plants that grow along Morib Beach, Malaysia. For identification of endophytic fungi, EF 4/ EF 3 and ITS 1/ ITS 4 PCR primer pairs were used to amplify the fungal 18S rDNA sequence and ITS region sequence, respectively. The resultant sequences were subjected to similarity search via the NCBI GenBank database. High-performance thin layer chromatography (HPTLC) hyphenated with bioassays was used to characterise the extracts in terms of their phytochemical profiles and bioactivity. Microchemical derivatisation was used to assess polyphenolic and phytosterol/ terpenoid content whereas biochemical derivatisation was used to establish antioxidant activities and α-amylase enzyme inhibition. The sulforhodamine B (SRB) assay was used to assess the anticancer effect of the extracts against HCT116 (a human colorectal cancer cell line). The present results indicated MBS 3.2 (Penicillium decumbens) as the most potent extract against HCT116 (IC50 = 0.16 μg/mL), approximately 3-times more potent than 5-flurouracil (IC50 = 0.46 μg/mL). Stepwise multiple regression method suggests that the anticancer effect of MBS 3.2 could be associated with high polyphenolic content and antioxidant potential. Nonlinear regression analysis confirmed that low to moderate α-amylase inhibition exhibits maximum anticancer activity. Current findings warrant further in-depth mechanistic studies.
  10. Teoh XY, Goh CF, Aminu N, Chan SY
    J Pharm Biomed Anal, 2021 Jan 05;192:113631.
    PMID: 33011581 DOI: 10.1016/j.jpba.2020.113631
    Atovaquone (ATQ) is a poorly soluble drug. Therefore, formulating ATQ into its supersaturated state through solid dispersion for bioavailability enhancement can be of great value. However, due to fast crystallising properties of ATQ, the quantification of ATQ in a supersaturated solid dispersion system can be complicated. Therefore, in pursuit of accurate quantification of such sample, a simple HPLC analytical method utilising a C18 column (250 × 4.6 mm ID, 5 μm) for the quantitation of ATQ has been developed and validated. Atovaquone elution using the proposed method demonstrated a retention time around 7.6 min with good linearity (R2 > 0.999). The system suitability is also detailed with the tailing factor at 1.365 ± 0.002. The addition of solubilising agent as sample treatment step aided in ensuring the accurate quantitation of the fast crystallising ATQ. The developed HPLC quantitation method has been successfully employed in the analysis of ATQ from solid dispersion samples in in vitro dissolution as well as ex vivo permeation studies for formulation development.
  11. Chen YL, Shi L, Agbo F, Yong SH, Tan PS, Ngounou Wetie AG
    J Pharm Biomed Anal, 2020 Oct 25;190:113493.
    PMID: 32795778 DOI: 10.1016/j.jpba.2020.113493
    A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the simultaneous quantification of apomorphine and its metabolites apomorphine sulfate and norapomorphine in human plasma for supporting clinical development of a novel apomorphine sublingual thin film (APL) for the treatment of Parkinson's disease. Analytes and internal standards (IS) were extracted from human plasma by Oasis HLB SPE cartridge, followed by a reversed phase LC-MS/MS analysis using multiple reaction monitoring (MRM) in positive mode (m/z 268 → 237 for apomorphine, 348 → 237 for apomorphine sulfate, and 348 → 237 for norapomorphine). Stable isotope-labeled compounds were used as IS for respective analytes. The validated curve ranges were 0.02-20 ng/mL, 10-1000 ng/mL, and 0.5-20 ng/mL for apomorphine, apomorphine sulfate and norapomorphine, respectively. Extraction recoveries were found to be 73.4 % (apomorphine), 81.1 % (apomorphine sulfate), and 58.6 % (norapomorphine). Established long-term plasma frozen storage stabilities were 504 days at -20 °C and276 days at -60 °C, respectively. The method has been successfully used for analyzing pharmacokinetics (PK) samples collected from a comparative bioavailability study of APL and the marketed apomorphine subcutaneous (s.c.) product Apo-go®. The results demonstrated that the 15-mg APL film administrated via sublingual produced comparable PK characteristics of apomorphine when compared to the commercial product Apo-go (2-mg) via s.c. administration, hence establishing the dose regimen for this sublingual formulation. It was also noticed that the sublingual 15-mg APL film produced a significantly higher apomorphine sulfate metabolite level than the 2-mg s.c. Apo-go, and both treatments yielded a negligible level of norapomorphine metabolite in humans.
  12. Romero Rocamora C, Ramasamy K, Meng Lim S, Majeed ABA, Agatonovic-Kustrin S
    J Pharm Biomed Anal, 2020 Jan 30;178:112909.
    PMID: 31618702 DOI: 10.1016/j.jpba.2019.112909
    A high-performance thin-layer chromatography (HPTLC) method combined with effect-directed-analysis (EDA) was developed to screen the antioxidant, neuroprotective and antidiabetic effects in essential oils derived from lavender flower, lemon myrtle, oregano, peppermint, sage, and rosemary leaves (Lamiaceae family). HPTLC hyphenated with microchemical (DPPH•, p-anisaldehyde, and ferric chloride) derivatizations, was used to evaluate antioxidant activity, presence of phytosterols and terpenoids, and polyphenolic content, while the combination with biochemical (α-amylase and acetylcholine esterase (AChE) enzymatic) derivatizations was used to asses α-amylase and AChE inhibitory activities. The superior antioxidant activity of oregano leaf extract is attributed to the presence of high levels of aromatic compounds, like polyphenolic acids. The strongest α-amylase inhibition was observed in lemon myrtle and rosemary plus extracts due to the presence of monoterpenes. Rosemary and sage extracts exhibit the highest AChE inhibition activity, with 1 μL essential oils being more potent than the recommended daily dose of donepezil. This superior neuroprotection was attributed to the presences of di- and triterpenes that displayed strong AChE inhibition and antioxidant potential in DPPH• free radical assay. Antioxidant activity was related to phenolic content (R = 0.49), while α-amylase inhibitory activity was positively related to antioxidant activity (R = 0.20) and terpenoid/sterol content (R = 0.31). AChE inhibitory activity was correlated (R = 0.80) to the combined effect of phenolics and terpenoids. Thus, the superior AChE inhibitory and neuroprotection potential of rosemary and sage essential oils could be attributed to joint effects of main phenolic and terpene constituents. The hyphenated HPTLC method provided rapid bioanalytical profiling of highly complex essential oil samples.
  13. Lah ZMANH, Ahmad SAA, Zaini MS, Kamarudin MA
    J Pharm Biomed Anal, 2019 Sep 10;174:608-617.
    PMID: 31265987 DOI: 10.1016/j.jpba.2019.06.024
    A facile electrochemical sandwich immunosensor for the detection of a breast cancer biomarker, the human epidermal growth factor receptor 2 (HER2), was designed, using lead sulfide quantum dots-conjugated secondary HER2 antibody (Ab2-PbS QDs) as a label. Using Ab2-PbS QDs in the development of electrochemical immunoassays leads to many advantages such as straightforward synthesis and well-defined stripping signal of Pb(II) through acid dissolution, which in turn yields better sensing performance for the sandwiched immunosensor. In the bioconjugation of PbS QDs, the available amine and hydroxyl groups from secondary anti-HER2 and capped PbS QDs were bound covalently together via carbonyldiimidazole (CDI) acting as a linker. In order to quantify the biomarker, SWV signal was obtained, where the Pb2+ ions after acid dissolution in HCl was detected. The plated mercury film SPCE was also detected in situ. Under optimal conditions, HER2 was detected in a linear range from 1-100 ng/mL with a limit of detection of 0.28 ng/mL. The measures of satisfactory recoveries were 91.3% to 104.3% for the spiked samples, displaying high selectivity. Therefore, this method can be applied to determine HER2 in human serum.
  14. Jirjees F, Soliman K, Wang Y, Sonawane R, Sheshala R, Jones D, et al.
    J Pharm Biomed Anal, 2019 Sep 10;174:145-150.
    PMID: 31167158 DOI: 10.1016/j.jpba.2019.05.038
    Bevacizumab is a full-length human monoclonal antibody used to treat various neovascular diseases such as wet age-related macular degeneration (AMD), diabetic eye disease and other problems of the retina. Monthly intravitreal injections of bevacizumab (Avastin®) are effective in the treatment of wet AMD. However, there is a growing demand in the development of sustained release ophthalmic formulations. Therefore, this study aims, for the first time, to develop a rapid, simple, and sensitive method using size exclusion chromatography coupled with fluorescence detection for routine quantification of bevacizumab in ophthalmic formulations and during in vitro release studies. The selected chromatographic conditions included an aqueous mobile phase composed of 35 mM sodium phosphate buffer and 300 mM sodium chloride (pH 6.8), a flow rate of 0.5 mL/min, and the fluorescence detector was operated at excitation and emission wavelengths of 280 and 340 nm, respectively. The peak area-concentration relationship maintained its linearity over concentration range of 0.1-20 μg/mL (R2 = 0.9993), and the quantitation limit was 100 ng/mL. The method was validated for specificity, accuracy, precision, and robustness. The developed method had a run time of 6 min at temperature 25 °C, making it a unique validated method for rapid and cost-effective quantification of bevacizumab.
  15. Saleem H, Zengin G, Ahmad I, Lee JTB, Htar TT, Mahomoodally FM, et al.
    J Pharm Biomed Anal, 2019 Jun 05;170:132-138.
    PMID: 30921647 DOI: 10.1016/j.jpba.2019.03.027
    The current research work was conducted in order to probe into the biochemical and toxicological characterisation of methanol and dichloromethane (DCM) extracts of Bougainvillea glabra (Choisy.) aerial parts. Biological fingerprints were assessed for in vitro antioxidant, key enzyme inhibitory and cytotoxicity potential. Total bioactive contents were determined spectrophotometrically and the secondary metabolite components of methanol extract was assessed by UHPLC mass spectrometric analysis. The antioxidant capabilities were evaluated via six different in vitro antioxidant assays namely DPPH, ABTS (free radical scavenging), FRAP, CUPRAC (reducing antioxidant power), phosphomolybdenum (total antioxidant capacity) and ferrous chelating activity. Inhibition potential against key enzymes urease, α-glucosidase and cholinesterases were also determined. Methanol extract exhibited higher phenolic (24.01 mg GAE/g extract) as well as flavonoid (41.51 mg QE/g extract) contents. Phytochemical profiling of methanol extract identified a total of twenty secondary metabolites and the major compounds belonged to flavonoids, phenolics and alkaloid derivatives. The findings of antioxidant assays revealed the methanol extract to exhibit stronger antioxidant (except phosphomolybdenum) activities. Similarly, the methanol extract showed highest butyrylcholinesterase and urease inhibition. The DCM extract was most active for phosphomolybdenum and α-glucosidase inhibition assays. Moreover, both extracts exhibited significant cytotoxic potential against five (MCF-7, MDA-MB-231, CaSki, DU-145, and SW-480) human carcinoma cell lines with half maximal inhibitory concentration values of 22.09 to 257.2 μg/mL. Results from the present study highlighted the potential of B. glabra aerial extracts to be further explored in an endeavour to discover novel phytotherapeutics as well as functional ingredients.
  16. Saleem H, Htar TT, Naidu R, Ahmad I, Zengin G, Ahmad M, et al.
    J Pharm Biomed Anal, 2019 Mar 20;166:128-138.
    PMID: 30640043 DOI: 10.1016/j.jpba.2019.01.007
    In this study, different solvent extracts (methanol, dichloromethane and n-hexane) from aerial and stem parts of Buxus papillosa C.K. Schneid (Buxaceae) were investigated for a panoply of bioassays. Biological profiles were established by determining antioxidant and enzyme inhibition profiles. Toxicity was tested using MTT cell viability assay on five different human cancer cell lines i.e, MCF-7, MDA-MB-231, CaSki, DU-145 and SW-480. For chemical fingerprinting, total bioactive contents and UHPLC-MS secondary metabolites profile were determined. Generally, both aerial and stem methanol extracts had highest total bioactive contents, radical scavenging and reducing power potential. DCM and n-hexane extracts were found to be most active for total antioxidant and metal chelating activity. The UHPLC-MS analysis of methanol extracts revealed the presence of several phenolic, flavonoid, alkaloid, saponin and depsipeptide derivatives. All the extracts were significantly active against butyrylcholinesterase, whereas moderate inhibition was observed for acetylcholinesterase, α-glucosidase and urease. Similarly, a considerable level of cytotoxicity was observed against all the tested cell lines with IC50 values ranging from 26 to 225.9 μg/mL. Aerial methanol and stem n-hexane extracts were found to be most cytotoxic. Principal component analysis was also performed to find any possible correlation between biological activities and total bioactive contents. On the basis of our findings, B. papillosa may be considered as promising source of bioactive molecules.
  17. Zahed FM, Hatamluyi B, Lorestani F, Es'haghi Z
    J Pharm Biomed Anal, 2018 Nov 30;161:12-19.
    PMID: 30142492 DOI: 10.1016/j.jpba.2018.08.004
    A highly efficient electrochemical sensor for the analysis of anticancer drug 5-fluorouracil (5-FU), is fabricated based on silver nanoparticles-polyaniline nanotube (AgNPs@PANINTs). AgNPs@PANINTs nanocomposite has been synthesized by a simple one-step method. Synthesized AgNPs@PANINTs nanocomposite was studied by Fourier transform infrared spectrometry, Scanning Electron Microscopy and Energy Dispersive X-ray. The fabricated PANINTs@AgNPs PGE was applied to the electrochemical sensing of 5-FU. Cyclic voltammetry and differential pulse voltammetry experiments illustrated high electro activity for the AgNPs@PANINTs nanocomposite. The study was explored using the Taguchi experimental design method. Electrochemical measurements using differential pulse voltammetry showed a wide linear relationship between 5-FU concentration and peak height within the range 1.0-300.0 μM with a low detection limit (0.06 μM). Also, the fabricated sensor showed excellent selectivity in the presence of two anticancer drugs and a number of other interfering compounds. The as-prepared sensor showed to be a promising device for a simple, rapid, and direct analysis of 5-FU.
  18. Mukhtar NH, Mamat NA, See HH
    J Pharm Biomed Anal, 2018 Sep 05;158:184-188.
    PMID: 29883881 DOI: 10.1016/j.jpba.2018.05.044
    A sample pre-treatment method based on a dynamic mixed matrix membrane tip extraction followed by capillary electrophoresis with contactless conductivity detection (CE-C4D) was evaluated for the determination of tobramycin in human plasma. The extraction tip device consisted of a cellulose triacetate membrane tip wall immobilised with 15% (w/w) of hydrophilic lipophilic balance (HLB) nanoparticles as adsorbent. The extraction was performed dynamically by withdrawing/dispensing the plasma sample through the tip device followed by desorption into 20 μL of acidified aqueous solution at pH 3 prior to the CE-C4D analysis. Under the optimum conditions, the detection limit of the method for tobramycin was 10 ng/mL, with intraday and interday repeatability RSDs of 3.5% and 4.5%, respectively. Relative recoveries in spiked human plasma were 99.6%-99.9%. The developed approach was successfully demonstrated for the quantification of tobramycin in human plasma samples.
  19. Khoo LW, Audrey Kow SF, Maulidiani M, Lee MT, Tan CP, Shaari K, et al.
    J Pharm Biomed Anal, 2018 Sep 05;158:438-450.
    PMID: 29957507 DOI: 10.1016/j.jpba.2018.06.038
    The present study sought to identify the key biomarkers and pathways involved in the induction of allergic sensitization to ovalbumin and to elucidate the potential anti-anaphylaxis property of Clinacanthus nutans (Burm. f.) Lindau water leaf extract, a Southeast Asia herb in an in vivo ovalbumin-induced active systemic anaphylaxis model evaluated by 1H-NMR metabolomics. The results revealed that carbohydrate metabolism (glucose, myo-inositol, galactarate) and lipid metabolism (glycerol, choline, sn-glycero-3-phosphocholine) are the key requisites for the induction of anaphylaxis reaction. Sensitized rats treated with 2000 mg/kg bw C. nutans extract before ovalbumin challenge showed a positive correlation with the normal group and was negatively related to the induced group. Further 1H-NMR analysis in complement with Kyoto Encyclopedia of Genes and Genomes (KEGG) reveals the protective effect of C. nutans extract against ovalbumin-induced anaphylaxis through the down-regulation of lipid metabolism (choline, sn-glycero-3-phosphocholine), carbohydrate and signal transduction system (glucose, myo-inositol, galactarate) and up-regulation of citrate cycle intermediates (citrate, 2-oxoglutarate, succinate), propanoate metabolism (1,2-propanediol), amino acid metabolism (betaine, N,N-dimethylglycine, methylguanidine, valine) and nucleotide metabolism (malonate, allantoin). In summary, this study reports for the first time, C. nutans water extract is a potential anti-anaphylactic agent and 1H-NMR metabolomics is a great alternative analytical tool to explicate the mechanism of action of anaphylaxis.
  20. Darwish NT, Sekaran SD, Alias Y, Khor SM
    J Pharm Biomed Anal, 2018 Feb 05;149:591-602.
    PMID: 29197806 DOI: 10.1016/j.jpba.2017.11.064
    The sharp increase in incidence of dengue infection has necessitated the development of methods for the rapid diagnosis of this deadly disease. Here we report the design and development of a reliable, sensitive, and specific optical immunosensor for the detection of the dengue nonstructural protein 1 (NS1) biomarker in clinical samples obtained during early stages of infection. The present optical NS1 immunosensor comprises a biosensing surface consisting of specific monoclonal NS1 antibody for immunofluorescence-based NS1 antigen determination using fluorescein isothiocyanate (FITC) conjugated to IgG antibody. The linear range of the optical immunosensor was from 15-500ngmL-1, with coefficient of determination (R2) of 0.92, high reproducibility (the relative standard deviation obtained was 2%), good stability for 21days at 4°C, and low detection limit (LOD) at 15ngmL-1. Furthermore, the optical immunosensor was capable of detecting NS1 analytes in plasma specimens from patients infected with the dengue virus, with low cross-reaction with plasma specimens containing the Japanese encephalitis virus (JEV) and Zika virus. No studies have been performed on the reproducibility and cross-reactivity regarding NS1 specificity, which is thus a limitation for optical NS1 immunosensors. In contrast, the present study addressed these limitations carefully where these two important experiments were conducted to showcase the robustness of our newly developed optical-based fluorescence immunosensor, which can be practically used for direct NS1 determination in any untreated clinical sample.
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