• Bulletin of the Korean Chemical Society
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• 제27권10호
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• pp.1604-1608
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• 2006

A simple and efficient cloud point extraction-spectrofluorimetric method for the determination of thiamine in human urine is proposed. The procedure is based on the oxidation of thiamine with ferricyanide to form thiochrome, its extraction to Triton X-114 micelles and spectrofluorimetric determination. The variables affecting oxidation of thiamine, extraction and phase separation were studied and optimized. Under the experimental conditions used, the calibration graphs were linear over the range 2.5-1000 ng $mL^{-1}$. The limit of detection was 0.78 ng $mL^{-1}$ of thiamine and the relative standard deviation for 5 replicate determinations of thiamine at 400 ng $mL^{-1}$ concentration level was 2.42%. Average recoveries between 93-107% were obtained for spiked samples. The proposed method was applied to the determination of thiamine in human urine.

• 분석과학
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• 제36권5호
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• pp.250-257
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• 2023

The development of a spectrofluorimetric method for the determination of trimethoprim according to the reaction between O-phthalaldehyde (OPA) in highly alkaline media, and 2-mercaptoethanol (2ME) and this reaction gives fluorescent product measured at (458) nm when excited at (342) nm. The optimization of the analytical parameters that influence intensity was investigated. The intensity of fluorescence of the formed product was linearly related to the concentration of trimethoprim in the (100-1200) ng mL^-1 range. The limit of detection and limit of quantification were estimated to be (22.54) ng mL^-1 and (75.15) ng mL^-1 respectively. The utility of the proposed methods was successfully verified by analysis of trimethoprim in pure and real pharmaceutical preparations with high accuracy, the recovery percentages Re%, were found to be (100.5) % and (99.76) % for pure drug and pharmaceutical preparations respectively.

• Bulletin of the Korean Chemical Society
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• 제27권8호
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• pp.1199-1202
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• 2006

A simple, sensitive and rapid spectrofluorimetric method was developed for determination of mefenamic acid in pharmaceutical preparation and human urine. The procedure is based on the oxidation of mefenamic acid with cerium (IV) to produce cerium (III), and its fluorescence was monitored at 354 nm after excitation at 255 nm. The variables affecting oxidation of drug were studied and optimized. Under the experimental conditions used, the calibration graphs were linear over the range 0.03-1.5 mg $L^{-1}$. The limit of detection was 0.009 mg $L^{-1}$ and the relative standard deviation for 5 replicate determinations of mefenamic acid at 1.0 mg $L^{-1}$ concentration level was 1.72%. Good recoveries in the range of 102-107 and 102-109% were obtained for pharmaceutical preparation and human urine, respectively. The proposed method was applied to the determination of MF in one pharmaceutical preparation and human urine. The amounts of mefenamic acid found are very similar to those obtained by a standard method.

• 분석과학
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• 제35권1호
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• pp.24-31
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• 2022

Herein, we present a simple, precise, accurate, and ultra-sensitive spectrofluorimetric method for estimation of clozapine (CLZ) in tablets and human plasma was developed and then validated. A highly fluorescent brown-yellowish fluorophore was formed (λ_ex=469 nm, λ_emi=540 nm) as a nucleophilic substitution reaction occurred between CLZ and 4-chloro-7-nitro-2,1,3-benzoxadiazole (NBD-Cl) in alkaline mcllavine buffer (pH 9.0). Optimum values of experimental parameters were carefully determined and optimized. The calibration curve was rectilinear over the concentration range of 80-900 ng mL^-1 with a linear correlation coefficient (r=0.9984). The LOD and LOQ were determined to be 14 ng mL^-1 and 42 ng mL^-1, respectively. The proposed approach has been used successfully to quantification of Clozapine in its commercial formulations and human plasma.

• 대한화학회지
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• 제58권2호
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• pp.227-229
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• 2014

• 분석과학
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• 제25권3호
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• pp.159-163
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• 2012

A spectrofluorimetric method has been developed for the determination of free $CN^-$ in real samples with fluorescent safranine-O. When safranine-O interacts electrostatistically with $CN^-$, the fluorescent intensity of safranine-O is decreased. Several experimental conditions such as pH of the sample solution and the amount of safranine-O were optimized. $Ag^+$ interfered higher than any other ions. Interference of $Ag^+$ could be disregarded because $Ag^+$ was scarcely contained or mostly complexed with $CN^-$ in selected real samples. With this proposed method, the linear range of $CN^-$ was from 5.0 to 110 ng/mL and the detection limit of $CN^-$ was 2.9 ng/mL. For validating this technique, real samples (Cu, Ag, Au electroplating wastewater, and untreated wastewater in university and in sewage treatment plant) were used. Recovery yields of 91.5%~106.0% were obtained. Based on experimental results, it is proposed that this technique can be applied to the practical determination of free $CN^-$.

• 분석과학
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• 제24권3호
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• pp.231-235
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• 2011

A spectrofluorimetric method for the determination of EDTA in real samples such as mayonnaise, powder detergent and cleansing cream with tiron (4,5-dihydroxy-1,3-benzenedisulfonic acid) as a fluorimetric reporter was developed. When tiron is chelated with Cu(II), the fluorescent intensity is decreased by a quenching effect. However, when Cu(II)-tiron chelate reacts with EDTA, fluorescent intensity is increased as tiron is released. Several experimental conditions such as pH of the sample solution, the amount of Cu(II), the amount of tiron, heating temperature and heating time were optimized. Fe(III) interfered more seriously than any other ions, interference of Fe(III) could be disregarded, because Fe(III) was scarcely contained in selected real samples. The linear range of EDTA was from $8.0{\times}106{-8}\;M$ to $2.0{\times}10^{-6}\;M$. With this proposed method, the detection limit of Fe(III) was $5.2{\times}10^{-8}\;M$. Recovery yields of 92.7~99.3% were obtained. Based on experimental results, it is proposed that this technique can be applied to the practical determination of EDTA.

• Bulletin of the Korean Chemical Society
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• 제28권2호
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• pp.246-250
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• 2007

The crude extract of kohlrabi (Brassica oleracea gongylodes) was prepared as a rich source of peroxidase and its enzymatic and specific activities in the presence of cross-linked polyvinylpyrrolidone as a stabilizer were determined. This extract was used to catalyze the oxidation of thiamine in the presence of hydrogen peroxide to thiochrome at pH 8.0. Thiochrome shows strong fluorescence at 436 nm with excitation at 370 nm. Based on the obtained results, a sensitive and simple spectrofluorimetric method was developed for the determination of thiamine. In the optimum conditions, the calibration graph was linear from 2 × 10-7 to 1 × 10-4 mol L-1, with a detection limit of 6.2 × 10-8 mol L-1. The relative standard deviation (RSD) was 1.2% for 5 × 10-6 mol L-1 thiamine. The method was successfully applied to the determination of thiamine in vitamin B1 and vitamin B complex tablets and vitamin B complex syrup.

• 응용화학
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• 제15권1호
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• pp.25-28
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• 2011

A highly sensitive spectrofluorimetric method was developed for the determination of levodopa based on the formation of a ternary complex with Eu³⁺ in the presence of ethylenediaminetetraacetic acid. It was found that this complex manifests intense fluorescence at 591 and 613 nm with excitation at 372 nm and maximum intensity was obtained at 613 nm. Under the optimum conditions, the enhanced fluorescence intensity was proportional to the concentration of levodopa over the range of 3×10^-9-2.5×10^-7 mol L^-1 with limit of detection (LOD) of 4.37×10^-10 mol L^-1. The method offers higher sensitivity and selectivity which could be effectively applied for the determination of levodopa in pharmaceutical and biological samples.

• Bulletin of the Korean Chemical Society
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• 제32권5호
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• pp.1777-1780
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• 2011