Methods for radiochemical and radionuclidic purity determination of some99mTc and113mIn radiopharmaceuticals

In order to determine the radiochemical impurities in pertechnetate solution as well as that of unbound^99mTc in its colloid and complex compounds, in indium chloride solution and related compounds, paper chromatography on Whatman No. 1, thin-layer chromatography on silica gel plates, and paper electrophoresis were applied. A simple method for the determination of radionuclidic purity was developed.     

Rapid determination of 90Sr/90Y in water samples by liquid scintillation and Cherenkov counting

Strontium-90 (⁹⁰Sr) is a ubiquitous contaminant at nuclear facilities, found at high concentrations in spent nuclear fuel and radioactive waste. Due to its long half-life and ability to be transported in groundwater, an accurate method for measuring ⁹⁰Sr in water samples is critical to the monitoring program of any nuclear facility. To address this need, a rapid procedure for sequential separation of Sr/Y was developed and tested in groundwater samples collected from an area of riverbed affected by a ⁹⁰Sr groundwater plume. Sixteen samples, plus spike and water blanks, were analyzed. Five different measurements were performed to determine the ⁹⁰Sr and yttrium-90 (⁹⁰Y) activities in the samples: direct triple-to-double-coincidence ratio (TDCR) Cherenkov counting of ⁹⁰Y, liquid scintillation (LS) counting for ⁹⁰Sr following radiochemical separation, LS counting for ⁹⁰Y following radiochemical separation, Cherenkov counting for ⁹⁰Y following radiochemical separation and LS counting of the Sr samples for ⁹⁰Y in-growth. The counting was done using a low-level Hidex 300SL TDCR counter. Each measurement method was compared for accuracy, sensitivity and efficiency. The results following Cherenkov counting and radiochemical separation were in very good agreement with one another.     

The radiochemical purity determination of18F preparations

A simple and fast chromatographic method for determining the chemical form of¹⁸F is given.     

Modified 2-window approach for rapid determination of 90Sr and 90Y at low quench level using liquid scintillation counting

⁹⁰Sr is a product of nuclear fission, the radioactivity of which can be determined by liquid scintillation counting (LSC). Because the LSC spectra of ⁹⁰Sr and its daughter ⁹⁰Y overlap each other, the following methods are usually used: (1) measuring immediately after ⁹⁰Sr/⁹⁰Y separation; (2) waiting to reach radioactive equilibrium; (3) adopting the conventional 2-window approach; and (4) using the spectra deconvolution technique. The first one requires ⁹⁰Sr/⁹⁰Y separation and immediate measurement; the second one is time-consuming; the third one is valid only for samples with the same quench level as the calibration standard; the last one is somewhat complicated, and in some cases it is not convenient to export the experimental data to some deconvolution software. Therefore, we have developed a modified 2-window approach to rapidly determine ⁹⁰Sr and ⁹⁰Y in either equilibrium or disequilibrium at low quench level. The key modification of the approach is to provide an LSC spectrum of pure ⁹⁰Y with the same quench level as the sample to be determined. This modification eliminates the need to conduct ⁹⁰Sr/⁹⁰Y separation for the sample itself, to prepare the quench curves, and to fit the LSC spectra with some deconvolution software.     

Improving the radiochemical purity determination of 123I-labeled metaiodobenzylguanidine

The HPLC method originally applied at the Nuclear Engineering Institute (IEN) for the radiochemical purity determination of ¹²³iodine labeled m-iodobenzylguanidine (¹²³I-mIBG) takes 18.5 min. The final product release also depends on this result, and to facilitate this stage, we aimed to decrease this analysis time. We also intended to use fewer toxic compounds, if feasible. The optimization approach used herein was a combination of factorial and mixture designs to study simultaneously the selected variables. Analysis time, resolution and chromatograms aspect were the measured responses. The qualitative analysis of these responses provided the best chromatographic separation conditions that were 52 mM KH₂PO₄ in a solution of ethanol and water (1:1), applying a flow rate of 0.50 mL min^?1 and C18 column (4.6 × 250 mm, 5 μm). These optimum conditions not only decreased the analysis time in 61 %, but also allowed the reduction of mobile phase toxicity. To assure reliable data, method validation was performed for these conditions. The method has proved its specificity, the detection limit found was 3.70 × 10^?4 MBq mL^?1 and the quantification limit has corresponded to 1.11 × 10^?3 MBq mL^?1. Repeatability and intermediate precision has not exceeded 3 and 5 %, respectively, and the accuracy has matched the interval of 95–105 %. This new method has been routinely applied in the radiochemical purity determination of ¹²³I-mIBG at IEN.     

The determination of241Pu by liquid scintillation spectrometry using the Packard 2250CA

The results of this study indicate that in terms of efficiency, the Packard 2250Ca liquid scintillation spectrometer is sensitive to the scintillation cocktail employed for²⁴¹Pu analysis, particularly when the burst counting circuit is enabled. Cocktails exhibiting low t-SIE values should be avoided since quenching has a critical influence on such a low energy ^– emitter. This effect would be independent of burst circuitry use. Cocktails which include naphthalene type derivatives such as the alkylnaphthalene solvent employed in Optiphase HiSafe 3 and Ultima Gold should be avoided since the broad pulse shapes produced are incompatible with the burst counting circuit which distinguishes background events from true ^– events by means of pulse shape/duration analysis. Efficiency is also sensitive to the concentration of bis-MSB employed in conjunction with the primary fluor. Enhancements in efficiency are observed with appropriate concentrations. These results are in line with previous work with¹⁴C and are postulated as being a consequence of sharpening prompt pulse widths or suppression of afterpulsing. It is recommended that Instafluor should be used to maximize response, or a cocktail such as butyl-PBD/bis-MSB in pseudocumene at rates of 6 and 1.5 mg ml^–1, respectively, where a lower vapor pressure solvent is particularly required.     

Fast determination of 90Sr using liquid scintillation counter based on shielding package

Journal of Radioanalytical and Nuclear Chemistry - A novel method for direct measurement of 90Sr in liquid samples was developed by using liquid scintillation counter. Based on the shielding...     

Standardization of 90Y solution by mean of a Cherenkov counting in comparison with a liquid scintillation counting technique

Journal of Radioanalytical and Nuclear Chemistry - This paper presents the standardization of 90Y solution using the Cherenkov method measuring in the TDCR counters. The counting efficiencies for...     

The use of liquid scintillation spectrometry as a very sensitive radioanalytical tool for the determination of alpha,beta and monochromatic electron emitting impurities in radiopharmaceutical compounds

Summary Many labeled compounds are used as radiopharmaceuticals (RP), for emission imaging and metabolic radiotherapy and contain as labeling agents γ, β^-, β⁺, monochromatic e^- and α emitting radionuclides (RN). These labeled compounds very often contain unexpected radionuclidic impurities. Some long-lived isotopic and non-isotopic impurities lead to undesirable radiation doses to the patient and his relatives, as well as to medical/paramedical personnel, other than the general population, due to rad-waste of contaminated specimen and excretion of biological fluids. Use was made of liquid scintillation counting/spectrometry (LSCS) for the detection of tiny amounts of charged particle emitting impurities in RPs labeled with ⁶⁴Cu, ⁶⁷Ga, ⁹⁰Y, ⁹⁰Sr/⁹⁰Y, ¹²³I, ¹⁵³Sm, ¹⁷⁷Lu and ²⁰¹Tl.     

Beta-spectroscopic separation of90Sr,90Y and89Sr with a scintillation detector

A -spectroscopic method for measurement of the isotope ratios and absolute activities of⁹⁰Sr,⁹⁰Y and⁸⁹Sr with an organic scintillator is described and tested. The correction factors for absorption in the sample and the detector window are calculated. The method can be used for rapid estimation of ratios and absolute activities of pure -emitters after a nuclear accident.Supported in part by the International Atomic Energy Agency, RC5633 and the National Fund for Scientific Research (Bulgaria).     

Fast liquid chromatographic determination of radiochemical and chemical purity of [11C]methionine by UPLC technique

Salinity, water logging, high nitrate, fluoride and dissolved uranium concentration in drinking water of southwest Punjab has impacted the local population leading to health issues and additional burden on economy. Though it was known that both U and its daughter products especially Rn contribute to radiological dose to the population through drinking water, there were no correlation studies carried out between these radioactive elements in U impacted regions of southwest Punjab. In this study, an initiative has been taken to assess the doses due to dissolved radon in drinking water. In addition, the U–Rn couple is evaluated in detail along with other hydrochemical parameters. The radon concentration ranges from 360–1700 Bq/m³ for Faridkot and 140–1400 Bq/m³ for Muktsar for both seasons and the related average total dose due to radon for both season of Faridkot and Muktsar are 9.79 µS/year and 7.74 µS/year respectively. The total dissolved uranium is in range of 16–350 µg/L for Faridkot and 14–106 µg/L for Muktsar for both seasons. An inverse correlation was observed between Rn and U, which could be attributed to diverse geochemistry of U and Rn in groundwater.

     

Development of a method for the determination of 226Ra by liquid scintillation counting

Liquid scintillation counting has not been widely applied to a-particle detection because of its poor energy resolution and variable background. In the present work, a time saving and reasonably accurate method for determination of ²²⁶Ra in water has been developed, using liquid scintillation spectrometry and pulse-shape analysis. The effect of three levels of chemical quench on the spillover of alpha interactions into the beta window and vice versa was assessed. The advantages of liquid scintillation in comparison with other methods (radon emanation) for determination of ²²⁶Ra are the high counting efficiency (~100%) and the easier sample preparation, with no need for sample preconcentration.     

Characterization and calibration of a large area beta scintillation detector for determination of Sr-90

A large area beta scintillation detector has been developed which is currently capable of determining Sr-90/Y-90 contamination in surficial soils. The detector system employs scintillating fiber optic arrays, with active dimensions approximately 15 cm wide by 100 cm long, both ends of which are coupled to multiple photomultiplier tubes (PMTs). Electronic processing includes coincidence requirements to optimize sensitivity and selectivity for the 2.28 MeV (maximum) beta particle from Y-90. Low energy beta particles and gamma rays are discriminated against using double ended and multi-layer coincidence requirements. The detector system is personal-computer-software controlled and data restored in a format compatible with standard database software for ease of final data reduction. Experimental calibration studies have shown a linear response for Sr-90/Y-90 soil concentrations from 12 to over 500 pCi/g and a discrimination factor of 50 to 1 versus Cs-137.Pacific Northwest Laboratory is operated for the U.S. Department of Energy by Battelle Memorial Institute under Contract DE-AC06-76RLO 1830.     

General principles of enzymatic methods and their use in the determination of the radiochemical purity of mono-and disaccharides labelled with14C

General principles of enzymatic methods for the determination of radiochemical purity of natural¹⁴C-mono-and-disaccharides are suggested, and analytical schemes using these principles have been worked out. The enzymatic method of determining the radiochemical purity of¹⁴C-glucose is given as an illustration.     

Rapid isocratic HPLC investigation of radiochemical purity for <Superscript>90</Superscript>Y-DOTATATE

DOTA-conjugated peptides, such as [DOTA⁰, Tyr³]ocreotide (DOTATOC) and [DOTA⁰, Tyr³]octreotate (DOTATATE) can be labeled with radionuclides such as ⁹⁰Y, ¹⁷⁷Lu and ¹¹¹In at high specific activities. These radiolabelled somatostatin analogues are used for peptide receptor radionuclide therapy (PRRT). Currently, radio-high performance liquid chromatography (radio-HPLC) and radio-thin layer chromatography (radio-TLC) are the methods of choice for the analysis of the labeled compounds. In literature, radiochemical purity of the radiolabelled DOTATATE was investigated using gradient reversed-phase radio-HPLC. However, these studies indicate long retention time of the radiolabelled compound of 14.52 min. In our study, a new simple and rapid reversed-phase isocratic system enables the radiochemical purity of the radiolabelled DOTATATE within a few minutes.     

The simple radiochemical determination of 90Sr in environmental solid samples by solvent extraction

Determination of ⁹⁰Sr in environmental solid samples is a challenging task because of the presence of so many other radionuclides in samples of interest. This problem was dealt with by radiochemical separation of strontium followed by yttrium separation and Cerenkov counting of the high-energy ??-particle emissions of ⁹⁰Y in order to quantitate ⁹⁰Sr. In this work, an improved method is described for the determination of ⁹⁰Sr in soil samples, through the separation of the daughter ⁹⁰Y at equilibrium. The procedure is based on the HDEHP solvent extraction in combination with liquid scintillation spectrometry (LSS). A low background Quantulus has been optimized for low level counting of Cerenkov radiation emitted by the hard ??-emitter ⁹⁰Y. The analytical quality of the method has been checked by analyzing IAEA Soil-375 reference materials. The analytical method has also been successfully applied to the determination of ⁹⁰Sr for moss-soil samples in inter-laboratory exercises through IAEA??s ALMERA network. The chemical recovery for ⁹⁰Y extraction ranged from 80 to 85% and the counting efficiency was 73% in the window 25?C400 keV.     

Synthesis of195mPt radiolabelled cis-diamminedichloroplatinum/II/ of high chemical and radiochemical purity using high performance liquid chromatography

An improved method is described for the synthesis of^195mPt-radiolabelled cis-diamminedichloroplatinum/II. An amount of 10 mg of 95% enriched¹⁹⁴Pt was irradiated for 75 h in the hydraulic conveyer of the KUR at a thermal neutron flux of approximately 8.15×10¹³ n.cm^–2.sec^–1 and the^195mPt-radiolabelled CDDP was purified using HPLC. The chemical yield is 61% its chemical purity is greater than 99.74% the radiochemical purity is nearly 100%, and the specific activity is 7.4×10⁶ Bq mg^–1 CDDP/200 Ci mg^–1 CDDP/.     

Liquid scintillation spectrometry of tritium in the investigation of compound adsorption at a water/nonpolar liquid interface

We examine the application of the scintillation phase method as a radiochemical assay for studying the behavior of surfactants in liquid/liquid systems. The theoretical background of the technique is described. Results of our investigation of cationic and nonionic surfactants in a water/organic liquid system (arenes, alkanes, alcohols) are summarized.     

Some theoretical aspects of the use of isotopic exchange in a heterogeneous liquid system for radiochemical separations

Theoretical possibilities of the application of isotopic exchange in a heterogeneous liquid system to the separation of radionuclides have been investigated. With certain simplifying assumptions, equations were derived which enable the calculation of both the separation efficiency and volume concentration for a one-stage separation process under static or dynamic conditions. The relations obtained can be used in the choice of an appropriate method for the separation and simultaneous enrichment of trace amounts of radionuclides from large-volume liquid samples by equilibrium isotopic exchange.