An electrochemical sensing platform with a molecularly imprinted polymer based on chitosan-stabilized metal@metal-organic frameworks for topotecan detection.

The present study aims to develop an electroanalytical method to determine one of the most significant antineoplastic agents, topotecan (TPT), using a novel and selective molecular imprinted polymer (MIP) method for the first time. The MIP was synthesized using the electropolymerization method using TPT as a template molecule and pyrrole (Pyr) as the functional monomer on a metal-organic framework decorated with chitosan-stabilized gold nanoparticles (Au-CH@MOF-5). The materials' morphological and physical characteristics were characterized using various physical techniques. The analytical characteristics of the obtained sensors were examined by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and differential pulse voltammetry (DPV). After all characterizations and optimizing the experimental conditions, MIP-Au-CH@MOF-5 and NIP-Au-CH@MOF-5 were evaluated on the glassy carbon electrode (GCE). MIP-Au-CH@MOF-5/GCE indicated a wide linear response of 0.4-70.0 nM and a low detection limit (LOD) of 0.298 nM. The developed sensor also showed excellent recovery in human plasma and nasal samples with recoveries of 94.41-106.16 % and 95.1-107.0 %, respectively, confirming its potential for future on-site monitoring of TPT in real samples. This methodology offers a different approach to electroanalytical procedures using MIP methods. Moreover, the high sensitivity and selectivity of the developed sensor were illustrated by the ability to recognize TPT over potentially interfering agents. Hence, it can be speculated that the fabricated MIP-Au-CH@MOF-5/GCE may be utilized in a multitude of areas, including public health and food quality.

Determination of Carnosic Acid by a Novel HPLC-UV Method in Human Plasma and Application to a Prototype Pharmacokinetic Study.

An HPLC method with UV detection was developed for the determination of carnosic acid in human plasma and applied to a pharmacokinetic study after oral administration of Rosemary extract to a healthy volunteer. Sample preparation depends on liquid-liquid extraction with hexane. Chromatographic separation was achieved with C18 column (150 mm × 4.6 mm × 5 µm), at 25°C with isocratic elution, mobile phase composed of solution A (methanol), and solution B (2% o-phosphoric acid in water) (90:10, v/v) at flow rate of 1.0 mL/min. The analyte was detected at 230 nm. The retention time is 4.20 ± 0.03 min. The method was validated in terms of accuracy, precision, specificity, robustness and detection and quantification limits, in accordance with European Medicines Agency guidelines. LOD and LOQ were found to be 0.075 and 0.25 ng/mL, respectively. The method was applied to the analysis of carnosic acid in human plasma with good recovery as 91.7%. The plasma concentration-time profile and pharmacokinetic parameters: AUC0-t, AUC0-∞, Cmax, tmax, t1/2 were calculated according to the assays. The method can certainly be used for routine analysis of carnosic acid in human plasma after oral administration of Rosemary extract, and for phase I clinical studies and bioavailability-bioequivalance studies as well.

Simultaneous determination of hydrochlorothiazide, amlodipine, and telmisartan with spectrophotometric and HPLC green chemistry applications.

For the quantifiable amounts of Telmisartan (TLM) and Hydrochlorothiazide (HYD) in the presence of Amlodipine (AML) in a ternary mixture of synthetic laboratory mixture, a novel, sensitive, quick, and practical reversed-phase high-performance liquid chromatography (RP-HPLC) method was given. In order to separate, a Waters Spherisorb ODS-2 C18 column was used. For HYD, TLM, and AML, these techniques were viable over linearity ranges of 4-12 µg/mL, 4-25 µg/mL, and 5-40 µg/mL, respectively. The mobile phase system was acetonitrile:methanol: phosphate buffer at pH 2.5 (65:5:30 v/v/v), and the flow rate was 1.5 mL/min. Novel spectrophotometric methods were applied for active substances to determine simultaneously. The first method is absorptivity centering using factorized spectrum, and the second method is dual amplitude difference coupled with absorbance subtraction. These approaches have been effectively applied to bulk, laboratory synthetic mixtures to employ active components quantitatively. Correlation coefficients were found to be higher than 0.99 and the limit of detection values lower than 0.49 µg/mL in both spectrophotometric methods. The methodologies were validated following ICH recommendations. In the developed HPLC method, the limit of detection values was found to be 0.01 µg/mL for HYD and 0.02 µg/mL for AML and TLM. The correlation coefficients for the HPLC method were found to be 0.9971 for HYD, 0.9990 for AML, and 0.9983 for TLM. The suggested HPLC technique is a simple, effective, sensitive, environmentally friendly, and time-saving approach for determining TLM and HYD in the presence of AML.

Determination of active ingredients in antihypertensive drugs using a novel green HPLC method approach.

A 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.

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.

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 (FE-SEM). 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 µmol/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.

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.

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.