Application of improved iodine–azide procedure for the detection of thiouracils in blood serum and urine with planar chromatography

Zakrzewski, Robert; Ciesielski, Witold

doi:10.1016/s1570-0232(02)00806-1

Cited by 18 publications

(11 citation statements)

References 7 publications

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“…The optimum conditions of the improved detection method using iodine-azide reaction for thiouracils were pre- sented in a previous report [19]. In this report, we have expanded the application of the method to the group of mercaptopyridines and mercaptopyrimidines and the influence of iodide ions on detection limits was checked.…”

Section: Detectionmentioning

confidence: 98%

“…The 4% sodium azide solution, pH 5.5 was applied to detect all thiols listed in Table 1 using iodine-azide reaction as a detection system. As in the previous report [19], the plates were exposed to iodine vapour for 5 s. This is the time within which iodine is adsorbed on the TLC plate. The exposure time is so short due to adsorption of iodine on the plate and vanishing of white spots.…”

Section: Detectionmentioning

confidence: 99%

“…The hampering effect of the iodide ions in iodine-azide reaction induced by many thiols or organothiophosphorus compounds is intensed with increasing iodide ions concentration [21]. In the previous report, the effect of potassium iodide concentration on detection limits was not examined [19]. According to the Kurzawa's report [22], an increase of potassium iodide concentration makes an increase of iodine consumption into iodine-azide reaction induced with mercaptopyrimidines and an increase of induction time.…”

Section: Influence Of Iodide Ions On Detection Limits Obtained With Imentioning

confidence: 99%

“…It offers a mean of selective and sensitive detection of thiols as inductors of the iodine-azide reaction. This method bases on visual observation of the plates after spraying with freshly prepared solution of sodium azide and starch and exposure to iodine vapour [19]. The spots become visible as white spots on a violet-grey background.…”

Section: Introductionmentioning

confidence: 99%

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Detection of mercaptopyridines and mercaptopyrimidines in planar chromatography with iodine–azide reaction as a detection system

Zakrzewski

Ciesielski

2005

Journal of Chromatography B

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Section: Detectionmentioning

confidence: 98%

Section: Detectionmentioning

confidence: 99%

Section: Influence Of Iodide Ions On Detection Limits Obtained With Imentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Detection of mercaptopyridines and mercaptopyrimidines in planar chromatography with iodine–azide reaction as a detection system

Zakrzewski

Ciesielski

2005

Journal of Chromatography B

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“…The reports of PTU determination in pharmaceutical preparations have mentioned the use of several separation methods, including HPLC with UV detection (AbdulFattah and Bhargava, 2001;Mitra et al, 2004) and TLC with iodine-azide reaction as a detection system (Zakrzewski and Ciesielski 2003).…”

Section: Introductionmentioning

confidence: 99%

Determination of propylthiouracil in pharmaceutical formulation by high-performance liquid-chromatography with a post-column iodine-azide reaction as a detection system

Zakrzewski

2008

Arch. Pharm. Res.

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A high-performance liquid chromatographic method with a post-column iodine-azide reaction has been chosen and tested for validity in quantitative determination of propylthiouracil in tablets. A mobile phase with a flow rate of 1.4 ml/min was conducted in the form of isocratic chromatography on a C18 column with acetonitrile-water-sodium azide solution (2.5%; pH 5.5) 24:26:50 (v/v/v). Unreacted iodine from post-column iodine-azide induced by reaction was monitored with visible detection at lambda=350 nm. The method proved both its linearity within the range of 8-100 nM (r2>0.9988) and satisfactory results of inter-day precision (RSD<4.2%) and accuracy (recovery>91%). The limits of detection (DDL) and quantification (DQL) reached the levels of 5 and 8 nM, respectively. The validation of the method comprised also its specificity. The results obtained proved the suitability and appropriateness of the suggested method for intended use.

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A novel approach for simultaneous determination of 2‐mercaptobenzimidazole and derivatives of 2‐thiouracil in animal tissue by gas chromatography/mass spectrometry

Liu

Zou

Xie

et al. 2007

Rapid Comm Mass Spectrometry

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A novel approach for determination of 2-mercaptobenzimidazole (MBI) and other thyreostatic residues in animal tissues by gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring mode was developed. The analytes in animal tissues (including hypothyroid, pork muscle and beef samples) were extracted by acetonitrile, and then purified by a matrix solid-phase dispersion (MSPD) procedure after the extraction residues had been dissolved in water. The thyreostatic residues were derivatized by pentafluorobenzyl bromide (PFBBr) under strong basic conditions and then N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) before GC/MS analysis. Different kinds of solid supports with various polarities for the MSPD procedure were investigated, and it was found that silica gel was suitable for the purpose. The average recoveries of the thyreostatic drugs in animal tissues ranged from 71.5-96.9% with the relative standard deviations below 10%. By using the developed method, the limits of detection were 10 microg/kg for MBI; 5 microg/kg for 6-phenyl-2-thiouracil; and 2 microg/kg for 2-thiouracil, 6-methyl-2-thiouracil and 6-propyl-2-thiouracil. The stability of the thyreostatic drugs in spiked animal tissues was tested, and the results showed that the thyreostatic drugs did not decompose within 3 months if the sample was stored in darkness below -20 degrees C.

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Application of improved iodine–azide procedure for the detection of thiouracils in blood serum and urine with planar chromatography

Cited by 18 publications

References 7 publications

Detection of mercaptopyridines and mercaptopyrimidines in planar chromatography with iodine–azide reaction as a detection system

Detection of mercaptopyridines and mercaptopyrimidines in planar chromatography with iodine–azide reaction as a detection system

Determination of propylthiouracil in pharmaceutical formulation by high-performance liquid-chromatography with a post-column iodine-azide reaction as a detection system

A novel approach for simultaneous determination of 2‐mercaptobenzimidazole and derivatives of 2‐thiouracil in animal tissue by gas chromatography/mass spectrometry

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