Improved Gas Chromatographic Determination of Guanidino Compounds Using Isovaleroylacetone and Ethyl Chloroformate as Derivatizing Reagents

Zounr, Rizwan Ali; Khuhawar, Muhammad Yar; Jahangir, Taj Muhammad; Alamgir, Malik

doi:10.2116/analsci.32.141

ANAL. SCI.

2016

DOI: 10.2116/analsci.32.141

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Improved Gas Chromatographic Determination of Guanidino Compounds Using Isovaleroylacetone and Ethyl Chloroformate as Derivatizing Reagents

Rizwan Ali Zounr

Muhammad Yar Khuhawar

Taj Muhammad Jahangir

et al.

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Cited by 3 publications

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References 31 publications

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“…Zounr et al have developed a gas chromatographic method for guanidino compounds using isovaleroylacetone and ethyl chloroformate as derivatization reagents. 15 The derivatization technique is also useful to develop an electrophoretic analysis. A traditional chromogenic derivatization reagent for a thiol group, 5,5′-dithiobis(2-nitrobenzoic acid), could be applied to develop a capillary electrophoresis with a UV detection method for aminothiols.…”

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Derivatization Techniques for Chromatographic Analysis

Kishikawa

2018

ANAL. SCI.

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Derivatization Techniques for Chromatographic Analysis

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2018

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GC Determination of Fluorouracil in Serum by Using Hexafluroroacetylacetone as Derivatizing Reagent

Zounr

Khuhawar

et al. 2022

Journal of Chromatographic Science

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A gas chromatographic (GC) procedure has been developed for the determination of fluorouracil (5-FU) after pre-column derivatization with hexafluoroacetylacetone. GC separation was from column DB-1 (30 m × 0.32 mm id) and the determination was by flame-ionization detection. The derivatization conditions were optimized at pH 4, heating at 90°C for 40 min and extraction of the derivative was in chloroform. Using the conditions nucleobases cytosine, uracil, thymine, adenine and guanine separated completely from fluorouracil. The linear calibration range and LOD for 5-fluorouracil were 0.5–40.0 and 0.2 μg/mL, respectively. The derivatization, elution and separation were repeatable in terms of retention time and peak height/peak area (n = 5) and relative standard deviations (RSD) were within 3.5%. The method was applied for the analysis of serum spiked with 5-FU with recovery of 95.5–97.5% with RSD 1.5–3.1%.

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GC Analysis of Metformin, Ranitidine and Famotidine from Pharmaceuticals and Human Serum

Zounr

Khuhawar

et al. 2023

Journal of Chromatographic Science

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A method has been designed based on gas chromatography with flame ionization detection (FID) for the separation and analyses of ranitidine, famotidine and metformin after pre-column derivatization with trifluoroacetylacetone and ethyl chloroformate. DB-1 (30 m × 0.32 mm id) column with film thickness 0.25 μm was used for the separation at an initial temperature of column was 100°C for 2 min, and ramping at 20°C/min up to 250°C, with a hold time of 3 min. The rate of nitrogen flow was 2.5 mL/min and FID was used for detection. Complete separation was obtained between all the three drugs including excess of derivatization reagents. Linear calibration curves and detection limits were obtained in the ranges 0.1–30 μg/mL and 0.011–0.015 μg/mL. The procedure was repeatable in terms of peak heights/peak areas and retention time (n = 5) for derivatization, quantitation and separation with relative standard deviations (RSDs) within 2.0–3.0%. The approach was examined for the analyses of drug products and serum after the intake of the drugs by healthy volunteers, and recoveries were obtained within 95–98% with RSDs 2.4–3.1%.

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Improved Gas Chromatographic Determination of Guanidino Compounds Using Isovaleroylacetone and Ethyl Chloroformate as Derivatizing Reagents

Cited by 3 publications

References 31 publications

Derivatization Techniques for Chromatographic Analysis

Derivatization Techniques for Chromatographic Analysis

GC Determination of Fluorouracil in Serum by Using Hexafluroroacetylacetone as Derivatizing Reagent

GC Analysis of Metformin, Ranitidine and Famotidine from Pharmaceuticals and Human Serum

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