Β-Cyclodextrin-Cross-Linked Polymer Microcolumn Dynamic Preconcentration/analysis for Trace Cadium

2011 ◽  
Vol 284-286 ◽  
pp. 82-86
Author(s):  
Xia Shi Zhu ◽  
Ying Gu ◽  
Ting Ting Hou
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Reference Material ◽  
Water Samples ◽  
Enhancement Factor ◽  
Optimum Conditions ◽  
Column Method ◽  
Relative Standard ◽  
Trace Cadmium

The adsorptive capability of β-Cyclodextrin-cross-linked polymer(β-CDCP) for cadmium was assessed in this work using column method. It was found that the complex (Cd(II)-5-Br-PADAP) could be quantitatively retained on the β-CDCP in the pH 8.5, eluted completely with 1.5 mol×L-1HCl. Under the optimum conditions, the linear range, detection limit (DL) and the relative standard deviation (R.S.D.) was 2.0-60.0 μg×L-1, 7.8 ng×L-1and 2.20% (n=3, c=20.0 μg×L-1) respectively. The separation of Cd(II) was achieved from water samples with an enhancement factor of 20. Moreover, the β-CDCP could be used repeatedly and offered better recovery. The method was validated using a certified reference material, and applied for the determination of trace cadmium in water samples.

Cloud Point Extraction-Fluorimetric Combined Methodology for the Determination of Magnolol

2013 ◽  
Vol 699 ◽  
pp. 34-39
Author(s):  
Li Liu ◽  
Xia Shi Zhu
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Cloud Point ◽  
Relative Standard Deviation ◽  
Cloud Point Extraction ◽  
Calibration Graph ◽  
Optimum Conditions ◽  
Relative Standard ◽  
Triton X

A new Triton X-114 cloud point extraction combined with fluorometry method for analysis of magnolol in drug samples was developed. Under the optimum conditions, the calibration graph was linear in the range of 2.0-150.0ng/mL of magnolol in the initial solution with r = 0.9998. Detection limit (DL) was 0.03ng/mL (S/N=3) and the relative standard deviation (RSD) for 20.0ng/mL of magnolol was 2.79%(n=11). The method was successfully applied for the determination of magnolol in drug samples with satisfactory results.

Spctrophotometric Determination of Trace Ruthenium by its Catalytic Effect on Oxidation of 3,5-DiBr-PADAP with KIO4

2012 ◽  
Vol 554-556 ◽  
pp. 1999-2005
Author(s):  
Zhi Rong Zhou ◽  
Qun Wang ◽  
Shu Yuan Zhang
Keyword(s):  
Activation Energy ◽  
Standard Deviation ◽  
Detection Limit ◽  
Catalytic Reaction ◽  
Oxidation Reaction ◽  
Catalytic Effect ◽  
Optimum Conditions ◽  
Potassium Periodate ◽  
Relative Standard

A spectrophotometric method for the determination of ruthenium (III) is described, based on its catalytic effect on the oxidation reaction of 2-[(3,5-dibromo-2-pyridy)azo]-5-diethylaminophenol (3,5-diBr-PADAP) with potassium periodate in 0.008 mol/L sodium hydroxide medium and in the presence of OP emulsifier (p-iso-octyl phenoxy polyethoxy ethanol) at 100 °C. The above reaction is followed spectrophotometrically by measuring the decrease in the absorbance at 530 nm for the catalytic reaction of 3,5-diBr-PADAP. The calibration curve for the recommended method was linear in the concentration range over 0.04 µg/L–1.0 µg/L and the detection limit of the method for Ru (III) is 0.012 µg/L. The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 100.48 kJ/mol. The relative standard deviation for the determination of ruthenium (III) at the concentration of 0.02 µg/25mL is calculated to be 2.30 % (n=11). In combination with distilled separation, the method has been successfully applied for the determination of trace ruthenium (III) in some ores and metallurgy products with the relative standard deviations (RSD) over 1.8 %–2.9 % and the recovery over 98.1 %–103.1 %.

scholarly journals Determination of Bentazone in Waters by Solid-Phase Spectrofluorimetry

1996 ◽  
Vol 79 (2) ◽  
pp. 567-570 ◽  
Author(s):  
José Luis Vilchez ◽  
Diego Torres-Bustos ◽  
Rosario Blanc ◽  
Alberto Navalón
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Relative Standard Deviation ◽  
Natural Water ◽  
Water Samples ◽  
Solid Phase ◽  
Excitation Wavelength ◽  
Relative Standard ◽  
Sensitive Method

Abstract A sensitive method for determining trace amounts of bentazone was developed. The method is based on solid-phase spectrofluorimetry. Bentazone was fixed on a dextran-type anion-exchange gel, and the fluorescence of the gel, packed in a 1 mm thick quartz cell, was measured directly at an excitation wavelength of 338 nm and an emission wavelength of 436 nm by using a solid-phase attachment. The applicable concentration range was 2.0–120.0 μg/L, with a detection limit of 0.4 μg/L. The relative standard deviation at the 30.0 μg/L level was 1.2%. The method was used to determine bentazone in natural water samples. Recoveries were 96.0–102.5%.

scholarly journals Spectrophotometric flow injection procedure to indirect determination of paracetamol in pharmaceutical formulations using o-tolidine as reagent

2018 ◽  
Vol 33 (2) ◽  
pp. 47
Author(s):  
Orlando Fatibello-Filho ◽  
Heberth Juliano Vieira
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Flow Injection ◽  
Pharmaceutical Formulations ◽  
Injection Method ◽  
Indirect Determination ◽  
Analytical Curve ◽  
Relative Standard ◽  
Injection Procedure

A spectrophotometric flow injection method for the determination of paracetamol in pharmaceutical formulations is proposed. The procedure was based on the oxidation of paracetamol by sodium hypochloride and the determination of the excess of this oxidant using o-tolidine dichloride as chromogenic reagent at 430 nm. The analytical curve was linear in the paracetamol concentration range from 8.50 x 10-6 to 2.51 x 10-4 mol L-1 with a detection limit of 5.0 x 10-6 mol L-1. The relative standard deviation was smaller than 1.2% for 1.20 x 10-4 mol L-1 paracetamol solution (n = 10). The results obtained for paracetamol in pharmaceutical formulations using the proposed flow injection method and those obtained using a USP Pharmacopoeia method are in agreement at the 95% confidence level.

scholarly journals Determination of Niacin in Infant Formula by Solid-Phase Extraction/Liquid Chromatography: Peer-Verified Method Performance–Interlaboratory Validation

2002 ◽  
Vol 85 (3) ◽  
pp. 654-664 ◽  
Author(s):  
Denis E LaCroix ◽  
Wayne R Wolf ◽  
G William Chase
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Reference Material ◽  
Infant Formula ◽  
Solid Phase ◽  
Phase Extraction ◽  
Relative Standard ◽  
Interlaboratory Validation ◽  
Extraction Liquid

Abstract This paper reports the results of the interlaboratory peer validation study of AOAC Peer-Verified Method (PVM) 1:2000 for the determination of niacin in infant formula by solid-phase extraction/liquid chromatography. We have used a Data Quality Objectives (DQO) approach to address not only method variability and robustness but also accuracy of data through the use of an appropriate reference material in conjunction with the interlaboratory validation study. Our DQO included the following: (1) statistical agreement of analytical results and quantitative recovery between 2 collaborating laboratories; (2) the repeatability relative standard deviation (RSDr) values and the HORRAT (Horwitz ratio) obtained (1.07), which satisfied the criteria of the Horwitz “limits of acceptability” at the analyte level present; (3) validation of lack of interference; and (4) accuracy agreement within assigned values for a certified reference material. National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1846 Infant Formula, with a certified value of 63.3 ± 7.6 μg/g for niacin content, was used as a test material for collaborative study and accuracy assessment. Niacin values obtained by the originating laboratory were 59.7 ± 4.0 μg/g (95% confidence interval [CI] = 1.4 μg/g with a relative standard deviation [RSD] of 6.7%) and by the peer laboratory were 56.6 ± 6.6 μg/g (95% CI = 4.1 μg/g, with an RSD of 11.7%). Statistical evaluation using the means equivalence test showed that nicotinic acid values obtained by the peer laboratory were equivalent to those values obtained by the originating laboratory. Linear calibration curves and quantitative recovery were obtained. Integration of the PVM process with a readily available certified reference material gives the user confidence in the accuracy of the data generated by the method through traceability to the reference material used.

A Study on Gadolinium Sensitized Chemiluminescence System

2012 ◽  
Vol 535-537 ◽  
pp. 1337-1340 ◽  
Author(s):  
Chi Yang ◽  
Nai Lin Ren
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Linear Relationship ◽  
Relative Standard Deviation ◽  
Optimum Conditions ◽  
Chemiluminescence Intensity ◽  
Experimental Conditions ◽  
Relative Standard

A new chemiluminescence system was built by using gadolinium as sensitizer, and the analysis capabilities of this system was tested as below. The method is based on chemluminescence of Ce (IV)-SO32- sensitized by Gd3+-OFLX. The effects of some critical experimental conditions were discussed and the optimum conditions for chemluminescence emission were investigated. The linear relationship between the relative chemiluminescence intensity and the concentration of OFLX is in the range of 2×10-9 g/mL～5×10-7 g/mL with a detection limit of 1.0×10-9g/mL .The relative standard deviation is 2.8% (n=11) for a level of 5.0×10-7 g/mL. The method has been applied to the analysis of OFLX in tablets with satisfactory results.

A method of high sensitivity and in situ determination of trace cobalt(II) in water samples with salicyl fluorone

2014 ◽  
Vol 70 (7) ◽  
pp. 1182-1187 ◽  
Author(s):  
Zhe Chen ◽  
Hua Li
Keyword(s):  
Flow Injection ◽  
Water Samples ◽  
High Sensitivity ◽  
Basic Solution ◽  
Optimum Conditions ◽  
Cetylpyridinium Bromide ◽  
Test Conditions ◽  
Relative Standard

Based on the sensitive reaction of Co(II) and salicyl fluorone with the presence of cetylpyridinium bromide in basic solution, a new method of flow injection micelle-solubilized spectrophotometry was developed for the determination of cobalt. The reaction was monitored for the absorbance of Co(II) at 540 nm. The reagents, flow injection variables and effects of foreign ions were investigated and the optimum conditions were established. At the optimum test conditions, the developed method provides a linearity range of 3–40 μg L−1 with a detection limit of 0.1 μg L−1 at about 60 h−1 sampling frequency. Relative standard deviation of 0.91, 0.95 and 0.89% were obtained for the determination of 3, 15 and 30 μg L−1 Co(II) solution. The proposed method has been successfully applied for analysis of trace amounts of cobalt in water samples.

scholarly journals Aqueous Two-Phase Systems: A New Approach for the Determination of Brilliant Blue FCF in Water and Food Samples

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Sabah Shiri ◽  
Tahere Khezeli ◽  
Shahram Lotfi ◽  
Sina Shiri
Keyword(s):  
Polyethylene Glycol ◽  
Standard Deviation ◽  
Food Samples ◽  
Brilliant Blue ◽  
Phase System ◽  
Optimum Conditions ◽  
Two Phase ◽  
Brilliant Blue Fcf ◽  
Relative Standard

A novel, simple, and more sensitive spectrophotometric procedure has been developed for the determination of brilliant blue FCF in water and food samples by an aqueous two-phase system (ATPS). In this method, adequate amount of polyethylene glycol/ sodium carbonate (PEG-4000/Na2CO3) was added to aqueous solution for formation of a homogeneous solution. To the mixture solution, suitable amount ofNa2CO3was added, the mixture solution was shaken until the salt was dissolved, and then it was separated into two clear phases easily and rapidly. The target analyte in the water sample was extracted into the polyethylene glycol phase. After extraction, measuring the absorbance at 634 nm was done. The effects of different parameters such as polyethylene glycol (type and concentration), pH, salt (type and amount), centrifuge time, and temperature on the ATPS of dye was investigated and optimum conditions were established. Linear calibration curves were obtained in the range of 0.25–750 ng/mL for brilliant blue FCF under optimum conditions. Detection limit based on three times the standard deviation of the blank (3Sb) was 0.12 ng/mL. The relative standard deviation (RSD) for 400 ng/mL was 3.14%. The method was successfully applied to the determination of brilliant blue FCF in spiked samples with satisfactory results. The relative recovery was between 96.0 and 102.2%.

Chemiluminescence Enhancement Effect for the Determination of Acetaminophen with the Catalysis of Manganese Deuteroporphyrin (Mn(III)DP)

2013 ◽  
Vol 575-576 ◽  
pp. 249-252 ◽  
Author(s):  
Ying Jun Chao ◽  
Liang Xiao Xie ◽  
Wei Cao
Keyword(s):  
Detection Limit ◽  
Pharmaceutical Preparations ◽  
Peak Height ◽  
Enhancement Effect ◽  
Optimum Conditions ◽  
Chemiluminescence Intensity ◽  
Relative Standard ◽  
Alkaline Conditions ◽  
Flow Injection Chemiluminescence

It is found thatManganese Deuteroporphyrin (Mn(Ⅲ)DP) can greatly enhance the chemiluminescence intensity of luminol-hydrogen peroxide system in alkaline conditions. Basing on that fact a flow injection chemiluminescence (CL) method has been developed for the determination of acetaminophen. With the peak height as a quantitative parameter applying optimum conditions, the relative CL intensity was linear with acetaminophen concentration in the range of 1.0×10-9～1.0×10-7 g/mL with a detection limit of 2.8×10-10 g/mL. The relative standard deviation (RSD) was 2.7% for 2.0 x10-8 g/mL acetaminophen (n = 11). The proposed method held low detection limit and was successfully applied to determination of acetaminophen in pharmaceutical preparations.

Iodometric determination of 2-mercaptobenzthiazole by coulometric titration

1982 ◽  
Vol 47 (2) ◽  
pp. 588-593 ◽  
Author(s):  
Zdeněk Kučera ◽  
Milan Karlík ◽  
Jiří Krofta
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Coulometric Titration ◽  
Optimum Conditions ◽  
End Point ◽  
Relative Standard ◽  
Standard Deviations

The optimum conditions were found for the determination of 2-mercaptobenzthiazole (MBT) by coulometric titration with the generated iodine using biamperometric indication of the titration end point. Use is made of the oxidation to the disulphide (n = 1) and to benzothiazole-2-sulphinate (n = 4) in the regions pH 4.5-8.5 and 10-12, respectively. Eight repeated titrations to the disulphide gave the relative standard deviations 0.27% and 1.23% in the determination of 1 675 and 33.5 μg MBT, respectively, seven repeated titrations of 419 μg MBT to benzothiazole-2-sulphinate afforded results with the relative standard deviation 0.34%.

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