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Summary

A stability-indicating gradient reverse-phase liquid chromatographic method was developed for the quantitative determination of process-related impurities and forced degradation products of oxcarbazepine in pharmaceutical formulation. The method was developed by using Inertsil cyano (250 × 4.6 mm) 5 μm column with mobile phase containing a gradient mixture of solvent A (0.01 M sodium dihydrogen phosphate, pH adjusted to 2.7 with orthophosphoric acid and acetonitrile in the ratio of 80:20 v/v) and B (50:40:10 v/v/v mixture of acetonitrile, water, and methanol). The flow rate of mobile phase was 1.0 mL min−1. Column temperature was maintained at 25°C and detection wavelength at 220 nm. Developed reverse-phase high-performance liquid chromatography (RP-HPLC) method can adequately separate and quantitate five impurities of oxcarbazepine, namely imp-A, imp-B, imp-C, imp-D, and imp-E. Oxcarbazepine was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Oxcarbazepine was found to degrade significantly in acid, base, and oxidative stress conditions. The degradation products were well resolved from oxcarbazepine and its impurities. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness.

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Summary

A simple, selective, and stability-indicating reverse phase liquid chromatographic method has been developed and validated for the simultaneous determination of impurities and forced degradation products of quetiapine fumarate. The chromatographic separation was achieved on Inertsil-3 C8, 150 mm × 4.6 mm, 5 μm column at 35°C with UV detection at 217 nm using gradient mobile phase at a flow rate of 1.0 mL/min. Mobile phase A contains a mixture of 0.01 M di-potassium hydrogen orthophosphate (pH 6.8) and acetonitrile in the ratio of 80:20 (v/v), respectively, and mobile phase B contains a mixture of 0.01 M di-potassium hydrogen orthophosphate (pH 6.8) and acetonitrile in the ratio of 20:80 (v/v), respectively. The drug product was subjected to the stress conditions of oxidative, hydrolysis (acid and base), hydrolytic, thermal, and photolytic degradation. Quetiapine fumarate was found to degrade significantly in acid, base, and oxidative stress conditions. The degradation products were well resolved from main peak and its impurities. The mass balance was found to be in the range of 96.6–102.2% in all the stressed conditions, thus proved the stability-indicating power of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: P. Sarita, G. Naga Raju, A. Pradeep, Tapash Rautray, B. Seetharami Reddy, S. Bhuloka Reddy, and V. Vijayan

Abstract  

Trace elemental imbalance in human beings is postulated to exert action, directly or indirectly, on the carcinogenic process. The objective of this study was to evaluate the levels of trace elements in blood sera of breast cancer patients and analyze their alteration with respect to healthy controls. This work was also intended to establish the role played by the trace elements in carcinogenic process. Particle induced X-ray emission (PIXE) technique was used for trace elemental analysis of blood sera of breast cancer patients and healthy controls. The PIXE measurements were carried out using a 2.5 MeV collimated proton beam from the 3 MV Tandem Pelletron accelerator at Institute of Physics, Bhubaneswar, India. On comparing the trace elemental content in the sera of breast cancer patients with those of control subjects, significant variations were observed in the levels of most of the trace elements. The serum levels of almost all the elements except Fe and Cu were observed to be depressed in cancer patients with respect to normal subjects. However, this variation was significant only for Ti (P < 0.00005), Cr (P < 0.005), Mn (P < 0.0005), Ni (P < 0.01), Zn (P < 0.000001), and Se (P < 0.05). On the other hand, significant elevations were observed in serum Fe (P < 0.05) and Cu (P < 0.005) levels in cancer patients. The findings presented in this paper give guidelines for future study into the possible roles and interactions of essential trace elements in the breast carcinogenic process.

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Summary

An isocratic ion-pair reversed phase high-performance liquid chromatography-ultraviolet (RP-HPLC-UV) method for analysis of eberconazole nitrate in bulk and in pharmaceutical dosage forms has been developed and validated. Best separation was achieved on Lichrospher C18 column (250 mm × 4.6 mm, 5 μm) using a mobile phase of 10 mM potassium dihydrogen phosphate containing 10 mM tetra-butyl ammonium hydroxide (pH adjusted to 2.8 with ortho phosphoric acid) and methanol (75:25, v/v) at a flow rate of 1.0 mL min−1. UV detection was performed at 220 nm. The method was validated for specificity, linearity, precision, accuracy, limit of detection, limit of quantification, robustness, and solution stability. The calibration plot was linear over the concentration range of 10–80 μg mL−1 (r 2 = 0.999) and the limits of detection and quantification were 0.3 and 0.9 μg mL−1, respectively. Intra-day and inter-day precisions were 1.13% and 1.67%, respectively. Experimental design was employed to optimize the method. The method was successfully used for analysis of eberconazole nitrate in commercially available cream (Ebernet).

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Abstract  

Boron concentration has been determined in groundwater samples, collected from Khuchch, Gujarat, India, by prompt gamma neutron activation analysis (PGNAA) after selective separation and pre-concentration by solvent extraction with 10% 2-ethyl hexane 1,3-diol in CHCl3. Solvent extraction separation helped to eliminate the interfering elements in PGNAA determination of boron. The sensitivity of PGNAA is found to be 18.83 cps/mg B based on the slope of a calibration plot obtained by carrying out measurements on synthetic boric acid samples containing boron in the range of 30–150 μg. Detection limit of the method is 0.2 μg/g counted for 35,000 seconds at a sample size of 15 gram. The precision (relative standard deviation at 1σ level) and accuracy of the method is 5%. The analytical results of the present method agreed well with well-established spectrophotometric determination of boron as boron-curcumin complex and inductively coupled plasma atomic emission spectroscopy (ICP-AES).

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Abstract  

Simultaneous measurement of gross alpha and gross beta activities by liquid scintillation counting technique using LKB Wallac Quantulus 1220 liquid scintillation counter (LSC) equipped with Pulse Shape Analyzer (PSA) is described. Three sets of pure alpha and pure beta standards simulating the activity concentration values of real samples in terms of α/β activity ratios were used to calibrate the LSC. Calibration methodology for the Quantulus 1220 with respect to the above measurements using 241Am and 90Sr/90Y standards of respective activity concentrations of ~25 dpm and ~104 dpm is described in detail. Also highlighted the need to calibrate the LSC using another set of 241Am and 90Sr/90Y standards of low and high activity concentrations respectively. The practicability and working performance of these calibration plots was checked by the validation trials with test samples spiked with 241Am and 90Sr/90Y covering range of α/β activity ratios from 1:1 to 1:50.

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Abstract  

Thorium along with its daughter products present in the soil is one of the major contributors to the external gamma dose in the environment. To establish the dose levels, quantification of thorium contents in soil samples is very important. As a part of pre-operational environmental radiological surveillance, a total of 23 soil and six sand samples were collected from different locations around the proposed nuclear power plant site of Jaitapur, Maharashtra. Thorium concentrations in these samples were determined by instrumental neutron activation analysis (INAA). Samples were irradiated with neutrons in Apsara reactor at a neutron flux of ~5 × 1011 cm−2 s−1 and radioactive assay was carried out using high resolution gamma ray spectrometry. Relative method of INAA was used for quantification of thorium utilizing 311.9 keV gamma ray of 233Pa, the daughter product of 233Th. The concentrations of thorium in the soil and sand samples were in the ranges of 4.0–18.8 and 1.2–6.2 mg kg−1 respectively.

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Abstract  

Direct determination of uranium in the concentration range of 8 μg L−1 to mg L−1 in water samples originating from different geochemical environments has been done using Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). Uranium detection with 2–3% RSD (relative standard deviation) has been achieved in water samples by optimizing the plasma power, argon and sheath gas flow. These parameters were optimized for three different emission lines of uranium at 385.958, 409.014 and 424.167 nm. Interference arising due to the variation in concentration of bicarbonate, sodium chloride, calcium chloride, Fe and dissolved organic carbon (DOC) on the determination of uranium in water samples was also cheeked as these are the elements which vary as per the prevailing geochemical environment in groundwater samples. The concentration of NaHCO3, CaCl2 and NaCl in water was varied in the range 0.5–2.0%; whereas Fe ranged between 1 and 10 μg mL−1 and DOC between 0.1–1%. No marked interference in quantitative determination of uranium was observed due to elevated level of NaHCO3, CaCl2 and NaCl and Fe and DOC in groundwater samples. Concentration of uranium was also determined by other techniques like adsorptive striping voltametry (AdSv); laser fluorimetry and alpha spectrometry. Results indicate distinct advantage for uranium determination by ICP-OES compare to other techniques.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: S. Abdul Sattar, B. Seetharami Reddy, V. Koteswara Rao, A. Pradeep, G. Naga Raju, K. Ramanarayana, P. Madhusudana Rao, and S. Bhuloka Reddy

Abstract  

Trace elemental analysis was carried out in various parts of 10 anti-epileptic medicinal plants using PIXE technique. A 3 MeV proton beam was used to excite the samples and spectra were recorded using a Si(Li) detector. Data analysis was done using Gupix Software. The elements Cl, K, Ca, Ti, Mn, Fe, Ni, Cu, Zn, Br and Sr were identified and their concentrations estimated. The presence of some of these trace elements is correlated with the anti-epileptic curative property of these plants.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: P. Geetha, N. Karunakara, Ujwal Prabhu, P. Ravi, J. Sudhakar, Nicy Ajith, K. Swain, R. Acharya, and A. Reddy

Abstract  

Instrumental and preconcentration methods of neutron activation analysis (NAA) have been standardized for the determination of concentration of iodine in grass and cow milk samples, respectively. To study the transfer of iodine from grass to milk, known quantity of grass spiked with potassium iodide solution was fed to a cow. The spiked grass samples and milk samples, obtained from the cow after the ingestion of spiked grass, were collected. Iodine was separated from the milk samples chemically using Dowex 1X8 anion exchange resin. Spiked grass and ion exchange resin samples were neutron irradiated and radioactive assay was carried out using a 45 % relative efficiency HPGe detector coupled to an 8k channel analyzer. Iodine concentrations in spiked grass samples were found to be in the range of 1,487–2,002 mg kg−1. Concentration of iodine in milk after 12 h of feeding the cow with spiked grass was 871 ± 56 μg L−1 which was reduced to 334 ± 32 μg L−1 after 48 h.

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