Propranolol In Urine Research Articles

Microextraction by packed sorbent of some β-blocker drugs with chitosan@mof-199 bio-composite in human saliva, plasma, and urine samples

The current study introduces microextraction by packed sorbent (MEPS) to extract three beta-blocker drugs (propranolol, atenolol, and betaxolol) from biological samples. The separation and detection of the drugs were performed by high performance liquid chromatography followed by UV detection. A green approach was applied for synthesizing chitosan@MOF-199 bio-composite, which was packed into the initial part of a metal spinal (22 gage). The effective parameters on the adsorption and desorption efficiencies, including sample solution pH, eluent flow rate, cycle numbers, type and volume of eluent solvent were evaluated and optimized. Under optimal conditions linear ranges (LRs = 5–600 µg L−1), limits of detection (LODs = 1.5–4.5 µg L−1), and relative standard deviations (RSDs% = 4.7 −5.3% with three replicates and concentration of 100 µg L−1) were obtained. Relative recoveries (RR%) for plasma (77–99%), saliva (81–108%), and urine (80–112%) samples were obtained. In this study, the drug release profile of propranolol in urine was evaluated. The results showed that the highest amount of propranolol is released 4 h after taking the drug. Based on the obtained results, this is an effective, fast, sensitive, reproducible, green, and user-friendly method for beta-blocker drug extraction in biological samples.

Water-compatible graphene oxide/molecularly imprinted polymer coated stir bar sorptive extraction of propranolol from urine samples followed by high performance liquid chromatography-ultraviolet detection

Due to the high selectivity and stability, molecularly imprinted polymers (MIPs) have been successfully applied in stir bar sorptive extraction (SBSE) as a special coating to improve the selective extraction capability for target analytes. However, traditional MIPs usually suffer from incompatibility in aqueous media and low adsorption capacity, which limit the application of MIP coated stir bar in aqueous samples. To solve these problems, a water-compatible graphene oxides (GO)/MIP composite coated stir bar was prepared in this work by in situ polymerization. The prepared water-compatible GO/MIP coated stir bar presented good mechanical strength and chemical stability, and its recognition ability in aqueous samples was improved due to the polymerization of MIP in water environment, the adsorption capacity for target analytes was also increased by the addition of GO in MIP pre-polymer solution. Based on it, a method of water-compatible GO/MIP coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detector (HPLV-UV) was proposed for the analysis of propranolol (PRO) in aqueous solution. The influencing factors of SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-UV method was evaluated under the optimized conditions. The limit of detection (LOD) of the proposed method for PRO was about 0.37μgL−1, and the enrichment factor (EF) was 59.7-fold (theoretical EF was 100-fold). The reproducibility was also investigated at concentrations of 5μgL−1 and the relative standard deviation (RSD) was found to be 7.3% (n=7). The proposed method of GO/MIP coating-SBSE-HPLC-UV was successfully applied for the assay of the interested PRO drug in urine samples, and further extended to the investigation of the excretion of the drugs by monitoring the variation of the concentration of PRO in urine within 10h after drug-taking.

HPLC column-switching technique for sample preparation and fluorescence determination of propranolol in urine using fused-core columns in both dimensions

A new and fast high-performance liquid chromatography (HPLC) column-switching method using fused-core columns in both dimensions for sample preconcentration and determination of propranolol in human urine has been developed. On-line sample pretreatment and propranolol preconcentration were performed on an Ascentis Express RP-C-18 guard column (5 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water (5:95, v/v) at a flow rate of 2.0 mL min(-1) and at a temperature of 50 °C. Valve switch from pretreatment column to analytical column was set at 4.0 min in a back-flush mode. Separation of propranolol from other endogenous urine compounds was achieved on the fused-core column Ascentis Express RP-Amide (100 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water solution of 0.5% triethylamine, pH adjusted to 4.5 by means of glacial acetic acid (25:75, v/v), at a flow rate of 1.0 mL min(-1) and at a temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 229/338 nm. A volume of 1,500 μL of filtered urine sample solution was injected directly into the column-switching HPLC system. The total analysis time including on-line sample pretreatment was less than 8 min. The experimentally determined limit of detection of the method was found to be 0.015 ng mL(-1).

Reusable phosphorescent probes based on molecularly imprinted polymers for the determination of propranolol in urine

The combination of the molecular imprinting techniques with room temperature phosphorescent detection was applied to the development of a simple and easy to regenerate probe for the determination of the beta-blocker propranolol in urine samples.First, bulk brominated polyurethanes were synthesized to ensure the applicability of the imprinting methodology with phosphorescent detection to the target molecule and then the polymerization was carried out onto glass slides to generate thin molecularly imprinted films. The analyte recognized by the imprinted-polymeric layer exhibited intense phosphorescence with a maximum at 520nm for an excitation wavelength of 314nm. Under optimized experimental conditions, the detection limit achieved was 22μg/L of propranolol, whereas the limit of quantification was 73μg/L of propranolol and the response was linear at least up to 1mg/L of propranolol. Finally, these reusable probes were successfully applied to urine samples analysis.

Simultaneous spectrofluorimetric determination of levodopa and propranolol in urine using feed-forward neural networks assisted by principal component analysis

The simultaneous determination of levodopa (LD) and propranolol (PRO) using fluorescence spectrometric technique is described. The method involves measuring the natural fluorescence of these drugs in the micellar media of sodium dodecyl sulfate (SDS) using principal component analysis-feed-forward neural networks (PC-FFNNs). Experimental conditions such as effect of pH and SDS concentration were optimized. Under the optimum conditions, the linear determination ranges of LD and PRO are 2.0 × 10 −8 to 1.0 × 10 −5 mol L −1 and 3.6 × 10 −9 to 1.8 × 10 −6 mol L −1, respectively. A set of synthetic binary mixtures of LD and PRO was prepared and their concentrations were predicted by the proposed method. Satisfactory results were obtained by the combination of fluorescence technique with chemometrics methods. The method was successfully applied to the determination of LD and PRO in tap water and in urine samples.

Direct determination of propranolol in urine by spectrofluorimetry with the aid of second order advantage

This work presented an application of the second-order advantage provided by parallel factor analysis (PARAFAC) aiming at direct determination of propranolol, a β-blocker also used as doping agent, in human urine by spectrofluorimetry. The adopted strategy combined the use of PARAFAC, for extraction of the pure analyte signal, with the standard addition method, for a determination in the presence of an individual matrix effect caused by the quenching action of the proteins present in the urine. The urine samples were previously 100 times diluted. For each sample, four standard additions were performed, in triplicates. A specific PARAFAC model was built for each triplicate of each sample, from three-way arrays formed by 231 emission wavelengths, 8 excitation wavelengths and 5 measurements (sample plus 4 additions). The models were built with three factors and always explained more than 99.87% of the total variance. The obtained loadings were related to PRO and two background interferences. The scores related to PRO were used for a linear regression in the standard addition method. The obtained determinations in the PRO concentration range from 5.0 to 20.0 μg ml −1 provided recoveries between 91.1 and 108.4%.

A sensitive fluorescence optosensor for analysing propranolol in pharmaceutical preparations and a test for its control in urine in sport

We describe a simple and selective method for analysing propranolol and a sensitive test for its control in urine. A flow-through fluorescence optosensor based on on-line immobilization in a non-ionic-exchanger (Amberlite XAD-7) solid support in a continuous flow was used in both cases. Determination was made in 5 mM H 2PO 4 −/HPO 4 2− buffer solution at pH 6 at a working temperature of 20 °C. Fluorescence intensities were measured at λ ex/em=300/338 nm with a response time of 80 s, thus obtaining a linear concentration range of between 0 and 250.0 ng ml −1 with a detection limit of 1.3 ng ml −1, an analytical sensitivity of 6.0 ng ml −1 and a standard deviation of 2.40% at a 150 ng ml −1 concentration level for propranolol. We also propose a test to detect propranolol in urine with a linear concentration range between 0 and 100.0 ng ml −1, a detection limit of 0.2 ng ml −1, an analytical sensitivity of 1.0 ng ml −1, and a standard deviation of 0.84% at a 75 ng ml −1 concentration level. The effect of proteins presents in urine samples were evaluated. The two proposed methods were satisfactorily applied to commercial formulations and urine samples respectively.

Fast determination of propranolol in urine and pharmaceutical preparations by stopped-flow and micellar-stabilized room-temperature phosphorescence: validation of the method

The stopped-flow mixing technique has been used to study the kinetic determination of propranolol by means of micellar-stabilized room-temperature phosphorescence. This mixing system diminishes the time required for the deoxygenation of micellar medium by sodium sulfite, allowing a kinetic curve that levels off within only 7 s to be obtained. The phosphorescence enhancers thallium (I) nitrate, sodium dodecyl sulfate, and sodium sulfite were optimized to obtain maximum sensitivity and selectivity. A pH value of 6.54 was selected as adequate for phosphorescence development. The kinetic curves of propranolol phosphorescence were scanned at λ ex=290 nm and λ em=524 nm. The calibration graphs were linear for the concentration range from 25 to 400 ng mL −1. The phosphorescence lifetime of propranolol is approximately 1210 μs. The detection limit calculated as proposed clayton was 13.53 ng mL −1 and by applying the error propagation theory, the detection limit was 8.37 ng mL −1. The repeatability was studied using 10 solutions of 200 ng mL −1 of propranolol; if error propagation theory is assumed, the relative error is 1.94%. The standard deviation for a replicate sample was 4.0 ng mL −1. This method was successfully applied to the determination of propranolol in commercial formulations and in urine. Suitable recovery values were obtained.

Studies on properties and application of non-protected room temperature phosphorescence of propranolol

A direct and simple non-protected room temperature phosphorimetry (NP-RTP) for determine propranolol, which using I − as a heavy atom perturber and sodium sulfite as a deoxygenator, has been developed. The phosphorescence peak wavelength maxima λ ex/ λ em=288/494, 522 nm. The analytical curve of propranolol gives a linear dynamic range of 8.0×10 −8–2.0×10 −5 mol l −1 and a detection limit of 3×10 −8 mol l −1. The influence of I − concentration on RTP lifetime of propranolol was studied and the luminescence kinetic parameters were calculated. It is found that the relation between I − concentration ( x) and RTP lifetime ( τ) can be expressed as τ=1.25e −0.477 x and the rate constants of phosphorescence emission k p was 0.800 per ms. The method was applied directly to determination of propranolol in urine and drug tablets with a satisfactory result. The recoveries were 96.6–97.4% and the relative standard deviation was 2% for the 1.00×10 −6–4.00×10 −6 mol l −1 propranolol in spiked urine sample.

Determination of drugs from urine by on-line immunoaffinity chromatography—high-performance liquid chromatography—mass spectrometry

A method for rapid extraction and identification of drugs in urine is described. The system utilizes a high-performance protein G immunoaffinity column coupled to a reversed-phase analytical column by use of a trapping column and switching valve. A small amount of antibody (5 μg drug-specific) is used for each analysis to extract either propranolol or lysergic acid diethylamide (LSD) from human urine. Urine diluted with phosphate-buffered saline is pumped directly through the protein G column thus eliminating time- and solvent-consuming sample preparation procedures. On-line ultraviolet or mass spectral analysis provides the means of drug detection and identification. With ultraviolet detection propranolol may be detected in spiked urine at the 250 pg/ml level. A Hewlett-Packard mass spectrometer modified for atmospheric pressure ionization and equipped with an ion spray source allows detection of propranolol in urine at 2.5 ng/ml and LSD at 500 pg/ml using single ion monitoring. The potential applicability of the technique for drug confirmations is discussed.

Optimization of selectivity in micellar chromatographic procedures for the determination of drugs in urine by direct injection

Selectivity was optimized for the determination of drugs in urine by direct injection micellar chromatography through changes in specific mobile phase parameters. The rôle of mobile phase pH and the type of surfactant used for mobile phase preparation was investigated. The retention of the urine matrix was found to be minimal between pH 5.5 and 7.5. The non-ionic surfactant, polyoxyethylene 23 lauryl ether (Brij 35), was found to be the surfactant of choice for the separation of drugs from urine. Favourable retention of both the urine background and the analyte was achieved with this surfactant. Micellar mobile phases of optimal composition were used to develop chromatographic procedures for the determination of furosemide, hydrochlorothiazide and propranolol in urine. Good accuracy (98-102% of drug recovered), precision (1-4% RSD) and linearity were obtained for all methods. Limits of detection for all drugs were adequate.