Validation and Comparison of Two Calibration Methods for the Measurement of Stable Iodine in the Urinary Matrix by ICP-MS:Standard Addition vs.External Calibration

Background: In the context of a nuclear reactor accident, thyroid is the main target organ of radioactive iodines. To avoid as much as possible thyroid disorders or even cancer development, it is recommended to administer a single dose of potassium iodide to people at risk of exposure. Nevertheless, the Fukushima Dai-ichi disaster has pointed out many questions about the conditions of stable iodine prophylaxis implementation highlighting the need for reflection further revision of the actual “iodine doctrine”. Therefore, providing useful data is required notably through the implementation of animal experiments to strengthen current knowledge and to edit new recommendations. Methods: Urinary iodine constitutes a very good indicator to investigate the function of thyroid, its interpretation demands reliable analyses. Prior to perform animal experiments, two calibration methods were designed by our lab and compared together (standard addition and external calibration) to assess the urinary concentration of stable iodine in urine by ICP-MS. They were validated based on several key parameters especially linearity, accuracy and limits of detection (LOD) and quantification (LOQ). Results: The results were nicely satisfying. Indeed, both calibration methods have indicated very good coefficients of correlations, accuracies with low expanded relative uncertainties were obtained. The estimated LOD in the sample for standard addition method and external calibration were fully acceptable, 0.39 μg·L-1 and 0.35 μg·L-1, respectively. All performance criteria have been thus fulfilled successfully. The established methods were proven to be accurate, robust and sensitive. Once validated, both calibration methods were applied to rat urine samples and the results of z-score and Wilcoxon W test concluded that there were no statistically significant differences between both methods.

Fast Determination of Phenanthrene in Soil by Gas Chroma- tography-Mass Spectrometry Using Chemometric Resolution and Standard Addition Method

A method for fast determination of the component in complex samples by using gas chromatography-mass spectrometry （GC-MS） was developed and used for quantitative analysis of phenanthrene in soils. In the method, window independent component analysis （WICA） was used for resolving the mass spectrum and non-negative im- mune algorithm （NNIA） was employed for obtaining the chromatographic profile. Therefore, spectral and chroma- tographic information of a specific component can be obtained from the measured GC-MS data of overlapping and high background. Six soil samples collected from different places were analyzed. The tedious pretreatments in pre- paring the samples and the elution in the separation were simplified for speeding up the analysis. Due to the com- plexity of the matrix, standard addition method was adopted for the final quantification. The applicability of the method was validated with a spiked sample and the results of the six samples are reasonable.

Quantification of trace amounts of impurities in high purity cobalt by high resolution inductively coupled plasma mass spectrometry

A An analytical method using high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS） for rapid simultaneous determination of 24 elements （Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn Sb, Ba, Pt, Au, and Pb） in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCI. The matrix effects because of the presence of excess HCI and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 ].tg·g^-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.

Determination of total sulfur in geothermal water by inductively coupled plasma-atomic emission spectrometry

Sulfur speciation and concentration in geothermal water are of great significance for the research and utilization of the water resources.In most situations,it is necessary to determine the total sulfur in geothermal water.In this study,the method was established for the determination of determining total sulfur content-the inductively coupled plasma-atomic emission spectrometry(ICP-AES),with the wavelength of 182.034 nm selected in spectral line of sulfur.It was identified that the optimal working conditions of the ICP-AES instrument were 1200 W for high frequency generator power 9 mm for vertical observation height,0.30 MPa atomizer pressure,and 50 r/min analytical pump speed.The matrix interference of the method was eliminated by the matrix matching method.Using this method,sulfur detection limit and minimum quantitative detection limit were 0.028 mg/L and 0.110 mg/L,respectively,whilst the linear range was 0.0-100.0 mg/L.The recovery rate of sample was between 90.67%and 108.7%,and the relative standard deviation(RSD)was between 0.36%and 2.14%.The method was used to analyze the actual samples and the results were basically consistent with the industry standard method.With high analysis efficiency,the method has low detection limit and minimum quantitative detection limit,wide linear range,good precision and accuracy,and provides an important detection method for the determination of total sulfur in geothermal water.

Application of RP-HPLC method in dissolution testing and statistical evaluation by NASSAM for simultaneous estimation of tertiary combined dosages forms

A dissolution method with robust high performance liquid chromatographic （HPLC） analysis for im- mediate release tablet formulation was developed and validated to meet the requirement as per Inter- national Conference on Harmonization （ICH） and United States Food and Drug Administration （USFDA） guidelines. The method involved the use of Agilent ZORBAX Eclipse XDB C18 column, and temperature was maintained at 30 ℃. After optimization, the mobile phase was selected as phosphate buffer （KH2PO4, 30 mM） ： ACN （60：40, v/v） with pH 3.0, and retention time Rt was found as 3.24, 4.16, and 2.55 min for paracetamol （PCM）, chlorpheniramine maleate （CPM） and phenylephrine hydrochloride （PH） respec- tively at 265 nm and at a flow rate of 1 mL/min. The relative standard deviation （%RSD） for 6 replicate measurements was found to be less than 2%. Furthermore net analyte signal standard addition method （NASSAM） with spectrophotometer was performed for standard and liquid oral suspension. On the basis of selectivity, sensitivity and accuracy analysis, it was confirmed that this novel method could be useful for simultaneous estimation of the given drug combinations. Two-way analysis of variance （ANOVA） was applied for evaluating the statistical difference between the assay results obtained via both NASSAM and RP-HPLC methods and ultimately no significant difference was found between both the methods. All the methods and results were acceptable and confirmed that the method was suitable for intended use.