Determination of tritium concentrations in humans before the development of a nuclear power plant in Turkey

The most widely used method to determine the level of tritium in humans is testing urine. Tritium concentrations in urine samples of 100 persons aged 18–66 years selected randomly from a pilot region in Turkey were analysed. The average activity concentration of urine samples was 4.66?±?1.94?Bq?L^?1 and the maximum activity concentration was 27.91?Bq?L^?1. The minimum detectable activity was 2.38?Bq?L^?1. The annual effective dose from tritium was also evaluated on the basis of the measurement results and reference values recommended by the International Commission on Radiological Protection. The effective doses for males and females were 4.56 and 3.54?nSv, respectively. These results were lower than the permissible annual effective dose for members of the public.     

Highly sensitive electrochemical detection of dopamine and uric acid on a novel carbon nanotube-modified ionic liquid-nanozeolite paste electrode

A novel biosensor has been constructed by incorporating modified nanosized natural zeolite and 3-hydroxypropanaminium acetate (HPAA) as a novel room temperature ionic liquid, supported on multiwalled carbon nanotube (MWCNTs) and employed for the simultaneous determination of dopamine (DA) and uric acid (UA). A detailed investigation by transmission electron microscopy and electrochemistry is performed in order to elucidate the preparation process and properties of the composites. The voltammetric studies using the modified carbon paste electrode show two well-resolved anodic peaks for DA and UA with a potential difference of 160 mV, revealing the possibility of the simultaneous electrochemical detection of these compounds. The modified carbon paste electrode shows good conductivity, stability, and extraction effect due to the synergic action of HPAA, MWCNTs, and iron ion-doped natrolite zeolite. Under optimized conditions, the peak currents are linear from 8.12?×?10^?7 to 3.01?×?10^?4?mol?L^?1 and from 9.31?×?10^?7 to 3.36?×?10^?4?mol?L^?1 with detection limits of 1.16?×?10^?7 and 1.33?×?10^?7?mol?L^?1 for DA and UA using the differential pulse voltammetric method, respectively. Finally, the modified carbon paste electrode proved to have good sensitivity and stability and is successfully applied for the simultaneous determination of DA and UA in human blood serum and urine samples.     

Development of an Optode for Detection of Trace Amounts of Hg2+ in Different Real Samples Based on Immobilization of Novel Tetradentate Schiff Bases Bearing Two Thiol Groups in PVC Membrane

A very sensitive and reversible optical chemical sensor based on a novel tetradentate Schiff base namely N.N^/bis(2-aminothiophenol)benzene-1,2-dicarboxaldehyde (ATBD) immobilized within a plasticized PVC film for Hg²⁺ determination is described. At optimum conditions (i.e. pH 6.0), the proposed sensor displayed a linear response to Hg²⁺ over 1.0?×?10^?10 ? 1.0?×?10^?2 mol L^?1 with a limit of detection of 7.23?×?10^?11 mol L^?1 (0.0145 μgL^?1). Moreover, the results revealed that, under batch condition, the sensor is fully reversible within a response time?~?35 s. In addition to its high stability and reproducibility, the sensor showed good selectivity towards Hg²⁺ ion with respect to common metal cations. The sensor was successfully applied for determination of Hg²⁺ ion in some real samples, including hair, urine and well water samples. The results were in good correlation with the data obtained using cold vapor atomic absorption spectrometry.     

Simultaneous Determination of Ritodrine and Isoxsuprine Using Coupling Technique of Synchronous Fluorimetry and H-Point Standard Addition Method

Simultaneous determination of two structurally related ß₂ adrenergic receptor agonists namely, Ritodrine HCl (RTH) and Isoxsuprine HCl (ISP) was performed using coupling technique of synchronous fluorimetry and H-point standard addition method. Under optimum conditions, linear determination ranges were 1.48 – 14.80?×?10^?6 mol L^?1 and 1.54 – 15.44?×?10^?6 mol L^?1 for ISP and RTH respectively. RTH and ISP could be determined simultaneously without interference from each other when their concentration ratio varies from 5:1 to 1:5 in the mixed sample. The proposed method was applied to the determination of RTH and ISP in synthetic mixture of pharmaceutical samples, the accuracy and precision of the results were satisfactory.     

A Validated Spectrofluorimetric Method for the Determination of Citalopram in Bulk and Pharmaceutical Preparations Based on the Measurement of the Silver Nanoparticles-Enhanced Fluorescence of Citalopram/Terbium Complexes

A simple, sensitive, and accurate spectrofluorimetric method was developed for the determination of citalopram in bulk and pharmaceutical preparations. The method is based on the enhancement of the weak fluorescence signal (FL) of the Tb (III)-citalopram system in the presence of silver nanoparticles. Fluorescence intensities were measured at 555 nm after excitation at 281 nm. Prepared silver nanoparticles (AgNPs) were characterized by UV-Visible spectra and transmission electron microscopy (TEM). Various factors affecting the formation of citalopram-Tb (III)-AgNPs complexes were studied and optimized. The fluorescence intensity versus concentration plot was linear over the range 0.02–14 μg?mL^?1, with an excellent correlation coefficient of 0.9978. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 7.15?×?10^?6?μg?mL^?1 and 2.38?×?10^?5?μg?mL^?1 respectively. The proposed method was found to have good reproducibility with a relative standard deviation of 3.66 % (n?=?6). The interference effects of common excipients found in pharmaceutical preparations were studied. The developed method was validated statistically by performing recoveries studies and successfully applied for the assay of citalopram in bulk powder and pharmaceutical preparations. Percent recoveries were found to range from 98.98 % to 100.97 % for bulk powder and from 96.57 % to 101.77 % for pharmaceutical preparations.     

Determination of Rosuvastatin in Urine by Spectrofluorimetry After Liquid–Liquid Extraction and Derivatization in Acidic Medium

Statins are a class of drugs mostly used for treating hyperlipidemia, and rosuvastatin is the newest drug in the market belonging to this class. In this present work, a method was developed based on the molecular fluorescence technique, with the objective to quantify rosuvastatin in urine samples. For this purpose, the study of several parameters was made to achieve the maximum analytical signal (under reaction with sulfuric acid during 40 min). Also, a previous step to avoid matrix interference was carried out (liquid–liquid extraction). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.38 and 1.28 mg L^?1, respectively. Linear relationship between rosuvastatin concentration and it’s fluorescence intensity was found until 5.0 mg L^?1. The proposed method was tested in several samples spiked with rosuvastatin and recovery was found in the range of 90?±?10 %.     

A Novel Method for the Assessment of Cortisol Hormone in Different Body Fluids Using A New Photo Probe Thiazole Derivative

A low cost and accurate method for the detection and analytical determination of the cortisol in pharmaceutical preparation, blood serum and urine was developed. The method was based upon the enhancement of fluorescence intensity of the band at 424 nm of the photo probe by different cortisol concentrations in acetonitrile at (pH 5.7, λ_ex?=?320 nm). The influence of the different parameters, e.g. pH, solvent, cortisol concentration and foreign ions concentrations that control the enhancement process of fluorescence intensity of the band of photo probe was critically investigated. The remarkable enhancement of the fluorescence intensity at 424 nm in acetonitrile by various concentrations of cortisol was successfully used as a photo- probe for the assessment of cortisol concentration. The calibration plot was achieved over the concentration range 8.0?×?10^?6–5.5?×?10^?9 mol L^?1 cortisol with a correlation coefficient of 0.998 and a detection limit of 4.7?×?10^?9 mol L^?1. The developed method is simple and proceeds without practical artifacts compared to the other determination methods.     

Excited state interaction between Hydrochlorothiazide and europium ion in PMMA polymer and its application as optical sensor for Hydrochlorothiazide in tablet and serum samples

This paper reports on a facile technique combined with a simple, sensitive and selective spectrofluorimetric method for the determination of hydrochlorothiazide. In methanol, at pH 8.3 and λ_ex=340, hydrochlorothiazide can remarkably enhance the luminescence intensity of the Eu³⁺ ion doped in polymethylmethacrylate polymer (PMMA) matrix. This could be due to the energy transfer from hydrochlorothiazide to Eu³⁺ in the excited stated. At the optimized experimental conditions, the enhancement of the characteristic emission band (617 nm) of Eu³⁺ ion doped PMMA is directly proportional to the concentration of hydrochlorothiazide with a dynamic range of 5×10^?8–1.0×10^?5 mol L^?1 and detection limit of 8.0×10^?9 mol L^?1. Application of the suggested method was successfully applied to the determination of hydrochlorothiazide in pharmaceutical preparations and human serum samples, with high percentage of recovery, good accuracy and precision.     

A sensitive amperometric detection of dopamine agonist drug pramipexole at functionalized multi-walled carbon nanotubes (f-MWCNTs) modified electrode

The electrochemical detection of dopaminergic agonist drug pramipexole dihydrochloride monohydrate (PPX) has been investigated by cyclic voltammetric (CV) and amperometric i–t techniques at functionalized multi-walled carbon nanotubes-modified glassy carbon electrode. For the first time, a sensitive and rapid electrochemical method was developed for the determination of PPX. The surface morphological characteristics of the proposed electrode have been studied by using transmission electron microscopy (TEM); further, electrochemical impedance spectroscopy (EIS) and Fourier transform infrared spectroscopy (FTIR) have been employed. PPX shows an irreversible anodic peak, which may be ascribed to the oxidation of the –NH groups of PPX. The proposed method was showing good sensitivity of 0.993 μA μM^?1 cm^?2 with a linear range of 5 to 340 μM by amperometric i–t and CV technique shows a linear range of 12.5 to 313 μM with a sensitivity of 1.92 μA μM^?1 cm^?2. The recovery of PPX from blood serum samples was found 100.6 and 98.9 %, respectively. Furthermore, the proposed method has been demonstrated for the determination of PPX in commercially available pharmaceutical samples and good agreement of results obtained.     

Application of extraction induced by emulsion breaking for trace multi-element determination in jet fuel by inductively coupled plasma-mass spectrometry

ABSTRACT

A novel method, based on extraction induced by emulsion breaking, is proposed for rapid simultaneous determination of iron, manganese, copper, and zinc in jet fuel by inductively coupled plasma-mass spectrometry. Several parameters affecting the extraction efficiency were investigated including the concentrations of nitric acid and emulsifying agents, centrifugal speed, and extraction time. The limits of detection for iron, manganese, copper, and zinc were 0.116, 0.028, 0.06, and 0.085 µg L^?1, respectively. The accuracy of the method was tested by the analysis of spiked samples (recovery percentages between 90% and 107% were observed) and by comparison with a well-established method.     

Novel nanostructured electrochemical sensor for voltammetric determination of N-acetylcysteine in the presence of high concentrations of tryptophan

A carbon paste electrode chemically modified with multiwall nanotubes and ethynylferrocene (ETFc) was used as a selective and sensitive electrochemical sensor for the determination of minor amounts of N-acetylcysteine (N-AC) in the presence of a high concentration of tryptophan (Trp). Square wave voltammetry (SWV) of N-AC at the modified electrode exhibited linear dynamic range with a detection limit (3 s) of 0.08 μmol?L^?1. The separations of anodic peak potentials of N-AC and Trp reached 400 mV using SWV. With good selectivity and sensitivity, the present method provides a simple method for selective detection of N-AC in real samples such as drug and urine.     

Validated HPLC-Fl Method for the Analysis of S-Adenosylmethionine and S-Adenosylhomocysteine Biomarkers in Human Blood

The natural methyl donor group, S-adenosylmethionine and its product, S-adenosylhomocysteine play an important role in many biochemical reactions involving transmethylation reactions. These compounds can be used as biomarkers in incipient diagnosis of various pathological disorders therefore the validation of a suitable method to routinely analysis of these compounds is very important. In this paper, a high performance liquid chromatrography method for S-adenosylmethionine and S-adenosylhomocysteine measurement as fluorescent 1,N ⁶-ethanoderivatives from biological samples was validated in terms of selectivity, linearity range of the response (R?>?0.9993), detection limit (9?×?10^?9 and 4.4?×?10^?9 molL^?1), the limit of quantitation (9.7?×?10^?9 and 5.7?×?10^?9?mol?L^?1), precision, trueness and robustness. The method for quantification simultaneous of these compounds is rapid, sensitive and precise and appropriate for clinical analysis.     

Fluorescence Determination of Azithromycin in Pharmaceutical Formulations by Using the Synchronous Scanning Approach After its Acid Derivatization

In this present work, a fluorescence method for azithromycin (9-deoxo-9a-aza-9a-methyl-9a-homoerythromycin) determination in pharmaceutical formulations is proposed. The method is based on the synchronous fluorescence (Δλ?=?30 nm, 482 nm) produced when azithromycin is derivatized in strong acidic medium (9.0 mol L^?1 HCl). The influence of the derivatization conditions (acid concentration, reaction time and temperature) was studied. Also, the possible reaction mechanism was discussed. In the optimized conditions, the method presented a limit of detection of 0.23 mg L^?1 and a limit of quantification of 0.76 mg L^?1. The developed procedure was successfully applied in the determination of azithromycin in pharmaceutical formulations.     

A fast and sensitive nanosensor based on MgO nanoparticle room-temperature ionic liquid carbon paste electrode for determination of methyldopa in pharmaceutical and patient human urine samples

In this study, we describe an ionic liquid–MgO nanoparticle modified carbon paste electrode (MgO/NPs/IL/CPE) was used as a simple, fast, and sensitive tool for the investigation of the electrochemical oxidation of methyldopa (MDOP) using voltammetric methods. The MgO/NPs was characterized with different methods such as TEM, SEM, and XRD. The oxidation peak potential of the MDOP at a surface of MgO/NPs/IL/CPE appeared at 450 mV that was about 100 mV lower than the oxidation peak potential at the surface of the traditional carbon paste electrode (CPE) under similar conditions. The electro-oxidation of MDOP occurred in a pH-dependent 2e^? and 2H⁺ process, and the electrode reaction followed a diffusion-controlled pathway. Under optimal conditions at pH 7.0, the anodic peak currents increased linearly with the concentration of MDOP in the range of 0.08–380 μmol L^?1 with a detection limit of 0.03 μmol L^?1 (3σ). The proposed sensor was successfully applied to the determination of MDOP in real samples such as drug and urine.     

Cloud point extraction-fluorimetric combined methodology for the determination of trace warfarin based on the sensitization effect of supramolecule

Compared to the fluorescence spectra of warfarin in pure ethanol and in the presence of the nonionic surfactant Tergitol 15-S-7 after cloud point extraction (CPE), it can be seen that the fluorescence emission peak underwent an obvious red shift and the fluorescence intensity of warfarin was significantly increased in the presence of Tergitol 15-S-7. In order to confirm Tergitol 15-S-7-induced supramolecular effects, the investigations on the fluorescence quantum yields of warfarin in the micellar medium and pure ethanol were performed. The experimental results showed that the supramolecular interactions between Tergitol 15-S-7 and the warfarin excimers played a key role for improving the warfarin fluorescence properties.Based on these facts, a simple fluorometric method combined with CPE for the determination of trace warfarin was developed for the first time. Under optimized experimental conditions, the linear concentration range for warfarin was 3.0×1.0^?9–1.0×10^?6 mol L^?1 and the detection limit was 3.3×10^?10 mol L^?1. And, the proposed method was approved to be appropriate for monitoring warfarin in actual pharmaceutical formulations and biological fluid samples by recovery test, in comparison with other reported methods being satisfactory.     

Luminescence enhancement effect for the determination of balofloxacin with balofloxacin-europium (III)-sodium dodecylbenzene sulfonate system

A novel method of luminescence enhancement effect for the determination of balofloxacin (BLFX) was proposed. A new system of the BLFX-Eu³⁺-SDBS (sodium dodecylbenzene sulfonate) was investigated. It was found that SDBS significantly enhanced the luminescence intensity of the BLFX-Eu³⁺ complex (about 20-fold). Under the optimized experimental conditions, the system exhibits an excellent linear relationship between the enhanced luminescence intensity and the concentration of BLFX over the range of 1.0×10⁻⁸-8.0×10⁻⁷ mol L⁻¹ with a correlation coefficient (R) of 0.9994, and the detection limit (3σ) of the method was determined as 2.0×10⁻⁹ mol L⁻¹. This method has been successfully applied for the determination of BLFX in pharmaceuticals and human urine/serum samples. Compared with most of the other methods reported, the rapid and simple procedure proposed in the text offers higher sensitivity, wider linear range, and better stability.     

Determination of Epinephrine in Pharmaceutical Formulation by an Optimized Novel Luminescence Method Using CdS Quantum Dots as Sensitizer

In this article, a novel chemiluminescence method using water-soluble CdS quantum dots (QDs) as sensitizers is proposed for the chemiluminometric determination of epinephrine. The method is based on the quenching effect of epinephrine on the chemiluminescence emission generated by the mixing of CdS quantum dots (QDs) with hydrogen carbonate (HCO₃ ^-) in the presence of hydrogen peroxide (H₂O₂) in an alkaline medium. The optimization of variables influencing the chemiluminescence response of the method has been carried out by using experimental design. Under the optimal conditions, there is good linear relationship between the relative chemiluminescence intensity and the concentration of epinephrine over the range of 5?×?10^?9–1?×?10^?6?molL^?1 with a 3σ detection limit of 5?×?10^?11?molL^?1. The method has been successfully applied to the determination of epinephrine in pharmaceutical formulation and the recovery test was done in human urine.     

Study on the Cofluorescence Effect of Europium (III)–Yttrium (III)–Balofloxacin–Sodium Dodecyl Sulfate System and Its Analytical Application

A new fluorescence enhancement phenomenon in the europium(III)–balofloxacin–sodium dodecyl sulfate system was observed when yttrium(III) was added. Based on this, a sensitive cofluorescence assay for the estimation of balofloxacin was established. Under the optimized conditions, the enhanced fluorescence signal was linear over the concentration of balofloxacin ranging from 3.0 × 10^?9 to 7.0 × 10^?6 mol L^?1 with a correlation coefficient of 0.9993. The detection limit (3 σ) was determined as 8.3 × 10^?10 mol L^?1. The presented method was successfully applied to determination of balofloxacin in pharmaceutical preparations, human serum, and urine. The possible fluorescence enhancement mechanism was also discussed.     

Cyclodextrin-functionalized magnetic graphene as solid-phase extraction absorbent coupled with flame atomic absorption spectrophotometry for determination of cadmium in water and food samples

A magnetic hydroxypropyl-β-cyclodextrin-functionalized reduced graphene oxide was synthesized and used as a magnetic solid-phase extraction adsorbent for the enrichment of cadmium from water and food samples before its determination by flame atomic absorption spectrometry. The effects of pH, amount of adsorbent, extraction time, desorption condition, and coexisting ions on the extraction efficiency were investigated and optimized. Under the optimal conditions, the limit of detection was 0.23?µg?L^?1 for water samples and 0.015?µg?g^?1 for food samples, respectively. The linear range was between 0.50 and 100.0?µg?L^?1 with a good correlation coefficient of 0.9986 in water samples, and between 0.050 and 5.0?µg?g^?1 with a correlation coefficient of 0.9975 in food samples. The method recoveries for the spiked samples were in the range of 87.5–102.4%, with the relative standard deviations ranging from 4.7% to 6.2% and enrichment factors ranging from 38 to 41, respectively. The adsorbent could be reused over 50 times without a significant change of extraction capability. The established method provides a promising environmentally friendly alternative for the determination of cadmium in complex matrix samples with no need of additional chelating reagents during the extraction process.     

Ultrasensitive fluorescent probe for copper ion based on cadmium selenide/cadmium sulfide quantum dots capped with dimercaprol

A new ultrasensitive copper ion fluorescent probe based on cadmium selenide/cadmium sulfide quantum dots capped with dimercaprol is described. Dimercaprol was bonded to the quantum dots through a surface ligand exchange to form dimercaprol-capped quantum dots whose fluorescence could be quenched by the coordination of dimercaprol on quantum dots’ surface with copper ion. The fluorescent probe based on dimercaprol-capped quantum dots showed a very good linear response range to copper ion from 0.1 to 50?µg?L^?1 with the detection limit of 0.087?µg?L^?1. The proposed method exhibited excellent sensitivity and selectivity due to the specific and strong affinity of dimercaprol with copper ion and the unique photoluminescence properties of quantum dots. The possible quenching mechanism was discussed and the probe was successfully applied to the determination of ultratrace copper in real samples.