Effect of the eluent composition in gel chromatography of99mTc (Sn)-methylene diphosphonate

Gel chromatography of^99mTc(Sn)-MDP on Sephadex has been performed by using the eluents of different composition and pH. Samples with constant ligand/reductant ratio were eluted by pure physiological saline as well as by saline which contained either the ligand only or both the ligand and the reductant. Their concentrations in the eluent were the same as those used in the preparation of the labeled complex.     

Quantitative analysis of solid mixtures by diffuse reflectance measurements

The factors affecting the reflectance of an absorbing substance mixed with material not absorbing at the wavelength of measurement were investigated and it was found that the effect of particle size could be eliminated by prolonged grinding. It is shown that the percentage by weight of the absorbing substance is directly proportional to the quantity (A/R)^1.383 (R = percentage reflectance ; A = 100 — R) and that this quantity is additive for 2 absorbing substances. A method is developed for the accurate determination of low concentrations of one and two absorbing substances mixed with non-absorbing material. The method is applicable to poorly crystallized substances which give no characteristic X-ray powder diffraction patterns as well as to crystalline solids. The reflectance of some substances is shown to be dependent on the previous history of the particular sample. The method is not applicable if there is physical interaction between the components of the mixture.     

Quantitative diffuse reflectance and transmittance spectroscopy of loosely packed powders

A self-consistent discontinuum theory describing the dependence of the diffuse reflectance and diffuse transmittance of powders on their optical absorp     

Quantitative investigation of matrices for diffuse reflectance infrared Fourier transform spectrometry

Five materials were investigated for use as diluent matrices for diffuse reflectance infrared Fourier transform (DRIFT) spectrometry of powdered samples. DRIFT spectra of powdered carbazole dispersed in germanium, silicon, diamond, potassium chloride and a chalcogenide glass were compared. Three particle size ranges were investigated for five concentrations of carbazole ranging from 0.1-10%. The effects of particle size and refractive index of the matrix are discussed.     

Quantitative determination of ochratoxin A in kidneys by liquid chromatography/mass spectrometry

A sensitive liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method for the quantitative determination of ochratoxin A (OTA) in kidney samples was developed. Ochratoxin B (OTB) was used as internal standard. Extraction of homogenized kidney samples was done by adding a chloroform/phosphoric acid mixture. Due to restriction of the sample size, less chloroform could be used than in previously described methods. Two different columns for clean-up were compared: strong anion exchange (Bond Elut SAX) and Extrelut NT columns. The high-performance liquid chromatography (HPLC) was used with gradient elution consisting of variable mixtures of formic acid (0.3%) in acetonitrile and formic acid (0.3%) in water. The mass spectrometer was operated in the positive ESI mode using multiple reaction monitoring. For OTA the precursor ion was m/z 404 while the product ions were at m/z 239 and m/z 341. For OTB the precursor ion was m/z 370 while the product ions were at m/z 205 and at m/z 324. A calibration curve of fortified kidney samples was used to quantify OTA. Method validation was performed according to Commission Decision 2002/657/EC. Decision limit (CCalpha), detection capability (CCbeta), precision, bias, trueness, specificity and measurement uncertainty were determined. In general, the best results were obtained using SAX clean-up. CCalpha and CCbeta were 0.11 and 0.25 microg kg(-1), respectively. Within-laboratory reproducibility (% CV) was 9, 9, and 5% for OTA-fortified kidney samples of 0.5, 1, and 2.5 microg kg(-1), respectively. Trueness (%) was 75, 69, and 57% for OTA-fortified kidney samples at 0.25, 0.5, and 1 microg kg(-1), respectively. Measurement uncertainty and expanded uncertainty were 14.85 and 29.70%, respectively. All criteria as laid down in Commission Decision 2002/657/EC were fulfilled. Therefore, this LC/ESI-MS/MS method can be used to monitor kidneys for OTA in the framework of Council Directive No. 96/23/EC.     

Preliminary study of quality control of99m Tc from99Mo generators

The separation of Tc(VII) from Mo(VI) by thin-layer and paper-chromatography is discussed. Some aspects concerning the formation and identification of lower oxidation states of Tc(VII) are also mentioned. Finally, a spot test is recommended for the determination of Mo(VI) and Al, which can be contaminants in the Tc(VII) solution eluted from the⁹⁹Mo column, filled with Al₂O₃.     

Adsorption and interface accumulation of aquasol and organosol carbon particles labeled with99mTc

Aerosol particles of^99mTc-labeled carbon were prepared by sublimation and introduced in various liquid media. The adsorption of the aquasol and organosol particles were studied for various adsorbing substances and media, with the effect of surface treatment and voltage application. The particles often accumulated at the aqueous-organic interface, and also on the vessel surface in the presence of both aqueous and organic phases. The distribution of the particles was examined by a gamma-camera for different organic phases under various concentrations of electrolytes in the aqueous phase.     

The stability of99mTc phosphorus compounds in plasma both in vivo and in vitro

The in vivo and in vitro stability of^99mTc hydroxyethlylidene diphosphonate, 99^mTc methylenediphosphonate and^99mTc pyrophosphate in plasma has been studied using paper chromatographic technique as the analytical tool. The results indicate that the amounts of^99mTc activity found both at the origin and R_f range of^99mTcO₄ ^? for in vivo experiments are slightly greater than those for either in vitro or control experiments. However, this amount of^99mTc activity represents about 0.16–0.4% of the injected dose. Therefore, it is suggested that^99mTc phosphorus radiopharmaceuticals are stable in vivo and neither oxidation nor hydrolysis of these bone imaging agents occurs in the blood.     

Simultaneous accumulation of both skeletal and appendage-based diversities on tandem Ugi/Diels-Alder products

Diversity-oriented organic synthesis (DOS) is a key concept for construction of skeletally diverse small molecule libraries to discover drug-like small molecules. Here, we describe a DOS class to transform a complex 7-oxanorbornene skeleton, which is readily accessible by a tandem Ugi/Diels-Alder reaction, into two heterotricycle skeletons selectively by using tandem ROM/CM/RCM reaction. In the present study, the mode of cyclization is pre-encoded by building blocks used in the complexity-generating tandem Ugi/Diels-Alder reaction. Since variable alkenes can be used in the CM reaction, our approach can be extended to construct both skeleton- and appendage-diverse small molecule libraries.     

Quantitative measurements of ammonium, hydrogenophosphate and Cu(II) by diffuse reflectance spectrometry

Diffuse reflectance spectrometry is shown to be useful for the quantitative determination of small amounts of pollutants. The relation between sample concentration and reflectance is described by the Kubelka-Munk equation. The experiments were performed with a laboratory constructed diode array spectrophotometer. We can obtain the quantitative reflectance values of different precipitates like ammonium with Nessler's reagent, hydrogenophosphate with silver nitrate and a complex such as Cu(II) with dithiooxamide 'rubeanic acid' by forming a spot colour on filter paper. We have obtained for each reagent a calibration curve by plotting the relative intensity of reflectance versus the log of the mol (dm(3))(-1) concentration. The linearity was obtained for Cu(II) from 8x10(-4) to 2.5x10(-2) mol l(-1) with r(2)=0.9838 and from 10(-3) to 10(-1) mol l(-1) for polyphosphate with r(2)=0.9975 and from 5x10(-4) to 5x10(-2) mol l(-1) for ammonium with r(2)=0.9889. We can consider that for a direct measurement of the intensity of reflectance, it is possible to perform quantitative spot-test analysis.     

Fundamental study of 99mTc nanocolloids for inflammation imaging

The biodistribution of nanometer-sized colloidal particles (nanocolloids, Solco-Basle Ltd.) was examined in six rabbits with turpentine-induced abscesses in the musculature of their hind legs. 99mTc labelled colloids with a mean particle size less than 100 nm were administered to each rabbit intravenously. The biodistribution of the tracer was studied with a gamma camera 1, 3, and 24 hours after injection. Prominent uptakes were demonstrated in the liver, spleen, bone marrow, kidneys, and urinary bladder. On the other hand, the abscess and surrounding inflammatory edema were depicted as unclearly margined faint hot spots. Subsequently, the rabbits were sacrificed and activity per gram tissues were counted with a well-type gamma counter. Although the results were almost in agreement with a gamma camera study, it was noticed the activity counts in the abscess were significantly higher than that of control muscles.     

Synthesis and preliminary study of 99mTc-mercaptoacetyl-triglycine (99mTc-MAG3) for radiolabeling of immune globulins

The synthesis of a complex molecule with its coordination center composed by a triamide monomercaptide tetradentate set of donor groups plus a phenyl-acetyl group as protector group of a sulphur atom is reported. This compound has been mixed with immune glubulin G, labeled with ^99mTc and purified by high resolution liquid chromathography (HRLC). The biological behavior of this labeled compound was evaluated with mice of Balb-C origin, showing the biological properties of a protein. This molecule might be another option for radio-immuno-scintigraphic analysis when using proteins of antigenic nature.     

Quantitative study of the photostability of spiropyrans

A quantitative method of determining the quantum yield of irreversible photodegradation (_C) of photochromic spiropyrans (SPP) was proposed for the first time. The _C of a large number of SPP of different types (with a different heterocyclic part) were determined. It was shown that for all of the SPP studied (except for dithiolane SPP), _C is almost independent of the heterocyclic part and is determined by the structure of the chromene part of the SPP. In addition to photodegradation, photooxidation takes place as a result of the reaction of the triplet state of the closed form of the SPP with O₂ for nitrosubstituted SPP of all types. The value of _C is determined by the efficiency of the reaction of isomer X of the colored form with the solvent or impurities, i.e., the lifetime of this isomer.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 2, pp. 290–298, February, 1990.     

Comparative study of quality control procedures for99mTc radiopharmaceuticals

Paper and TLC chromatographic methods have been evaluated for the control of the labeling and stability of eight Tc-radiopharmaceuticals. The different supporting media and eluents have been studied and the most suitable methods have been classified according to their usefulness, reliability and rapidity. Moreover the artefacts encountered have been investigated. Alumina is found not suitable for its interference with TcO ₄ ^– . Acetate buffer seems to be labeled by TcHR inducing frequently subsequent smearings. Methyl ethyl ketone is optimal for the quantification of TcO ₄ ^– except in Tc-HIDA. TcHR never migrates as well as Tc-S Coll, Tc-MAA and Tc-HSA. The well-defined separation of TcO ₄ ^– and TcHR from the radiopharmaceutical often requires a two-step method.Throughout this paper, the symbol Tc will be used to represent technetium-99m.