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Now showing 1 - 10 of 11
  • Publication
    Determination of active ingredients in antihypertensive drugs using a novel green HPLC method approach
    (2022-09-01T00:00:00Z) TIRIS, GİZEM; Mehmandoust, Amirhossein; Karimi, Fatemeh; ERK, NEVİN; TIRIS, GİZEM
    © 2022 Elsevier LtdA novel, sensitive, fast, and pratic RP-HPLC methods were presented for the quantitative amounts of Telmisartan (TEL) and Olmesartan (OLM) in the presence of Amlodipin (AML) in a binary mixture of pharmaceutical preparation. Waters Spherisorb ODS-2 C18 column was used for separation. These methods were valid over linearity ranges of 2.5–30 μμg/mlL, 2–85 μμg/mlL, and 2–35 μμg/mlL for OLM, TEL, and AML, respectively. The mobile phase system consisted of acetonitrile:methanol: phosphate buffer at pH 3.0 (65:5:30 v/v/v), and the flow rate was 1,5 mlL/min for OLM and AML. The mobile system-s other mixture (TEL and AML) was acetonitrile:methanol: phosphate buffer at pH 2.5 (65:5:30 v/v/v), and the flow rate was 1,5 mlL/min. These procedures were successfully applied to bulk, laboratory synthetic mixture, and medicinal dosage forms to use active ingredients quantitatively. The studied methods were validated according to ICH guidelines. In the developed HPLC method, the limit of detection values was found to be 0.020 μμg/mlL for TEL, 0.025 μμg/mlL for OML, and 0.070 μμg/mlL for AML. The correlation coefficients for the HPLC method were found to be 0.9938 for TEL, 0.9996 for OML, and 0.9982 for AML. The calibration range is between 2.5 and -30, 5–35, and 2–85 μμg/mlL for OLM, AML, and TEL, respectively. The proposed HPLC method is a convenient, effective, sensitive, green, and time-saving method for the rapid determination of TEL and OLM in the presence of AML.
  • Publication
    High performance liquid chromatographic analysis of lercanidipine in human breast milk
    A simple, rapid, precise and accurate isocratic reversed phase HPLC method was developed and validated for the determination of lercanidipine hydrochloride in pharmaceutical tablets and spiked human breast milk. The chromatographic separation was achieved on C18 (250x4.6 mmx5 mu m) column using a mobile phase consisting of acetonitrile and phospate buffer (pH=4) (55:45, v/v) at a flow rate of 1.1 mL/min and UV detection at 237 nm. The linearity of the proposed method was investigated in the range of 1.0-40 mu g/mL (r(2)=0.9990). The method was validated in terms of accuracy, precision, reproducibility, specificity, robustness, and detection and quantification limits, in accordance with ICH guidelines. The proposed method is found as suitable for routine quantification of lercanidipine in human breast milk.
  • Publication
    A novel stability-indicating method for determination of a new antidepressant effect of vortioxetine in a pharmaceutical formulation by using RP-HPLC
    (2020-12-01T00:00:00Z) TIRIS, GİZEM; Alver, Cansu; ERK, NEVİN; TIRIS, GİZEM
    Background: A novel rapid, accurate, and stability-indicating reversed-phase high performance liquid chromatographic (RP-HPLC) and first derivative spectrophotometric determination were explained for the assay of vortioxetine (VRT) in bulk and pharmaceutical formulations. For RP-HPLC method, optimal separation and determination of VRT were achieved with a Waters Symmetry C-18, (100 x 4.6 mm, 3.5 mu m) analytical column using a mobile phase consisting of methanol:0.05 M potassium dihydrogen phosphate (pH:3.0 +/- 0.05) (30:70, v/v) in isocratic mode with flow rate of 1.3 mL min(-1). Injection volume was 20 mu L. The maximum absorption wavelength of VRT is 225.0 nm; hence, 225.0 nm was studied as the detection wavelength and column at 50 degrees C temperature. The caffeine was used as the internal standard (IS). On the other hand, the first derivative spectrophotometric method for the analysis of vortioxetine was performed by measuring the amplitude at 251.7 and 272.6 nm.
  • Publication
    A sensitive voltammetric sensor for specific recognition of vitamin C in human plasma based on MAPbl(3) perovskite nanorods
    (2022-01-01T00:00:00Z) TIRIS, GİZEM; Khoshnavaz, Yasamin; Oven, Elif Naz; Mehmandoust, Mohammad; ERK, NEVİN; TIRIS, GİZEM
    A novel and sensitive electrode was suggested for the rapid determination of ascorbic acid (AA) using a glassy carbon electrode (GCE) modified with synthesized MAPbl(3) and L-cys (L-cys/MAPbl(3)/GCE). Determination of ascorbic acid as an important component of the human diet due to help in decreasing blood pressure and improving endothelial function is crucial. The synthesized MAPbl(3) was characterized by different methods, including transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and X-ray diffraction (XRD). The fabricated electrode exhibited superior electrical conductivity and fast electron transfer kinetics. The results illustrated that the developed electrode had an outstanding electrocatalytic activity towards the oxidation of AA in 0.1 M Britton-Robinson buffer(B-R) as a supporting electrolyte. The modified electrode demonstrated a linear range in differential pulse voltammetry of 0.02-11.4 mu M with a low detection limit of 8.0 nM for ascorbic acid. It can be stated that the proposed sensor can be successfully applied to the determination of ascorbic acid in human plasma samples.
  • Publication
    A New HPLC Method with UV Detection for the Determination of Carnosol in Human Plasma and Application to a Pharmacokinetic Study
    This article aims to present a simple and sensitive, HPLC-UV method, which was developed to determine carnosol in human plasma samples. Chromatographic separation was achieved with C18 column (150 mm x 4.6 mm x 5 mu m), at 25 degrees C with gradient elution of the mobile phase consisting of methanol-water (2% o-phosphoric acid) at flow rate 1.2 mL/min. The analyte was detected at 230 nm by UV detector. The retention time of carnosol is 3.40 +/- 0.01 min. This currently developed method was validated according to ICH criteria by evaluating the specificity, linearity, precision, accuracy and robustness. The method was determined to be linear in a concentration range of 1-20 ng/mL with the correlation coefficient of 0.9942. The proposed method was applied successfully to the analysis of carnosol in spiked human plasma with good recovery as 96.4% and the precision of the method was determined by intra day and interday assays with the highest RSD % values 5.71. The method successfully applied to a pharmacokinetic study with determination of C-max, t(max), t(1/2) and AUC, by administration of carnosol to a healthy volunteer.
  • Publication
    Ultra fast liquid chromatographic analysis of nonsteroidal anti-inflammatory drugs with fluorimetric detection in tap water, urine, and pharmaceutical samples
    (2022-06-01T00:00:00Z) Onal, Cem; TIRIS, GİZEM; Tekkeli, Evrim Kepekci; Onal, Armagan; TIRIS, GİZEM; TEKKELİ, ŞERİFE EVRİM
    A novel analytical method based on ultra-fast liquid chromatography using fluorimetric detector was developed and validated for determination of non-steroidal anti-inflammatory drugs (NSAIDs) (ibuprofen (IBP), etodolac (ETD), dexketoprofen (DKP), sodium diclofenac (SDCF), and naproxen (NPX) in tap water, urine and pharmaceutical samples. Precolumn derivatisation of targeted NSAIDs was carried out with 4-bromomethyl-7-methoxy coumarin (BrMmC) using dibenzo-18-crown-6-ether as reaction catalyst leading to the formation of a fluorescent compound. The obtained fluorescent compound of NSAIDs were measured at excitation wavelength as 325 nm, and emission wavelength of 395 nm. Optimum analytical conditions were carefully studied and improved. C18 column, with the dimensions of 4.0 x 100 mm and 3 mu m particle size, was used. Gradient elution with methanol: water 40:60; v/v (eluent A) and acetonitrile 100% (eluent B) were used as mobile phase and flow rate of 0.4 mL/min. The linearity range of the analytes were between 0.01-10.0 mu g mL(-1). Recovery values obtained from pharmaceutical preparations were found as 100.04%, 99.99%, 100.09%, 99.98% and 100.47% for IBP, ETO, DKP, SDCF, NPX, respectively. LOD values were found to vary between 0.00009 mu g mL(-1) and 0.00048 mu g mL(-1) in tap water, urine and pharmaceutical samples. The optimised technique was successfully applied for the determination of NSAIDs in tap water, urine, and pharmaceutical specimen. The specified NSAIDs were not found in real tap water samples.
  • Publication

    A reusable and sensitive electrochemical sensor for determination of idarubicin in environmental and biological samples based on NiFe2O4 nanospheres anchored N-doped graphene quantum dots composite; an electrochemical and molecular docking investigation

    (2022-09-01T00:00:00Z) Mehmandoust, Mohammad; Pourhakkak, Pouran; TIRIS, GİZEM; Karimi-Maleh, Hassan; ERK, NEVİN; TIRIS, GİZEM
    An ultrasensitive and selective voltammetric sensor with ultra-trace level detection limit is introduced for idarubicin (IDA) determination in real samples. The as-synthesized nanocomposite was characterized by several techniques, including Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy, Energy-dispersive X-ray spectroscopy (EDX), and Field emission scanning electron microscopy (FESEM). The electrocatalytic performance of the developed electrode was observed by cyclic voltammetry (CV), differential pulse voltammetry (DPV), electrochemical impedance spectroscopy (EIS), and chronoamperometry. The limit of detection (LOD) of the developed sensor for idarubicin is 1.0 nM, and the response is found to be in the dynamic concentration range of 0.01-1.9 mu mol/L in a Britton-Robinson buffer (B-R, pH = 6.0). Moreover, the fabricated electrode illustrated high selectivity with good repeatability and reproducibility for diagnosing idarubicin as an anthracycline antileukemic drug. Furthermore, to evaluate the validity of the recommended method, three real samples, including human plasma, urine, and water samples, were analyzed with satisfactory recovery and compared with high-performance liquid chromatography (HPLC). The minor groove-binding mode of interaction was also supported by docking simulation studies, emphasizing that IDA can bind to ds-DNA preferably and confirmed experimental results. The reduced assay time and the possibility of measuring a single sample with another anticancer drug without any interference are significant advantages compared to the HPLC. The developed and validated sensor could be a valuable point-of-care diagnostic tool for IDA quantification in patients.
  • Publication
    (2022-01-01T00:00:00Z) TIRIS, GİZEM; Tekkeli, S. Evrim Kepekci; Önal, Cem; Ceylan, Burhan; ÖNAL, Armağan; TIRIS, GİZEM
    © 2022, Publishing House of the Romanian Academy. All rights reserved.This research presents a new, sensitive and selective UPLC method with fluorometric detection for the determination of sorafenib in human plasma and application of the method to a pharmacokinetic study. Sorafenib was precolumn derivatized with 7-chloro-4-nitrobenzofurazan (NBD-Cl) and the separation of the fluorescent derivative was performed with a C18 column (50 mm x 2.1 mm, 1.7 µm) at 40ºC using a mobile phase composed of acetonitrile-0.1% trifluoroacetic acid in water (60:40, v/v) by isocratic elution with flow rate of 0.5 mL min−1. The injection volume was 7 µL. The method depends on the measurement of the derivative using fluorescence detection (λex = 398 nm, λem = 425 nm). The retention time of sorafenib was 3.10 ± 0.02 min. The novel method was validated in accordance with ICH criteria by studying on the parameters such as specificity, linearity, precision, accuracy and robustness. The method was determined to be linear in a concentration range of 0.25-10 µg mL−1 with the correlation coefficient of 0.9995. Limit of detection and quantitation were found to be 0.075 and 0.25 µg mL−1, respectively. Intraday and interday RSD values were less than 5.48%. The plasma concentration–time profile and pharmacokinetic parameters such as AUC0–t, AUC0–∞, Cmax, tmax, t1/2 were measured according to the assays. The proposed method is feasible to investigate the bioequivalence and bioavailability and routine analysis of the drug in plasma.
  • Publication
    The power of High Impact Amplitude Manipulation (HIAM) technique for extracting the basic spectra of two Fixed-dose combinations (FDC) -Spectrophotometric purity analysis via spectral contrast angle
    (2022-05-15T00:00:00Z) Saleh, Sarah S.; Lotfy, Hayam M.; TIRIS, GİZEM; ERK, NEVİN; El-Naem, Omnia A.; TIRIS, GİZEM
    © 2022 Elsevier B.V.HIAM technique allows the extraction of the original constant signal of each single component out of interference signals of a mixture and further transformed into basic spectrum (D0). It includes the methods: ratio subtraction coupled with unified constant subtraction (RS-UCS), constant center (CC) and constant extraction (CE). The technique was introduced for the analysis of two pharmaceutical formulations used to treat cardiovascular diseases. The formulations are binary combinations of Amlodipine (AML) with either Atorvastatin (ATR) or Candesartan (CND) which shows interefernce absorbance signals. The technique was valid over the linearity range of (5.0–35.0 µg/ml) for AML, ATR and CND with recovery percentage 100.40 ± 1.88, 100.00 ± 0.86 and 99.83 ± 1.07, respectively. The extracted signals were tested for its purity by spectral contrast angle (cos θ) to illustrate the efficency of the HIAM technique where cos θ values ranges from (0.9902 to 0.9986). The presented technique was fully validated regarding ICH guidelines and were statistically compared using one-way ANOVA at 95% confidence.
  • Publication
    Determination of dihydrocapsaicin adulteration in dietary supplements using LC-MS/MS
    (2020-01-01T00:00:00Z) DİNCEL, DEMET; Olgan, Hatice; Canbaloglu, Zeynep; Yalcin, Sule; Erkucuk, Aysen; TIRIS, GİZEM; GÖREN, AHMET CEYHAN; DİNCEL, DEMET; TIRIS, GİZEM; GÖREN, AHMET CEYHAN
    Adulterations of dietary supplements are serious threats to public health in all around of world. Nowadays, in order to obtain the intended effect from natural remedies, the adulteration of natural products via artificial or harmful chemicals are increasing. A rapid LC-MS/MS method for determination of capsaicin and dihydrocapsaicin in dietary supplements via Fortis C18 (150 x 3 mm; 3 mu m) column at 25 degrees C was developed and validated in a mixture of mobile phase A (1 % formic acid solution and 0.1 % ammonium formate in water) and B (1 % formic acid solution and 0.1 % ammonium formate in methanol) with gradient program at a flow rate of 0.35 mL/min. The recoveries of developed methods weytre obtained in the range of % 95.4-106.3 for capsaicin and % 96.3-108.9 for dihydrocapsaicin. This study shows that synthetic compound dihydrocapsaicin is widely use in dietary supplements products for adulteration to increase the effects of product without any declaration.