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

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  • ZOUNR Rizwan Ali
    Institute of Advanced Research Studies in Chemical Sciences, University of Sindh
  • KHUHAWAR Mumammad Yar
    Institute of Advanced Research Studies in Chemical Sciences, University of Sindh
  • JAHANGIR Taj Muhammad
    Institute of Advanced Research Studies in Chemical Sciences, University of Sindh
  • ALAMGIR Malik
    Institute of Advanced Research Studies in Chemical Sciences, University of Sindh

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An improved GC method in terms of sensitivity and decrease in the analysis time has been developed for the analysis of eight guanidino compounds: guanidine (G), methylguanidine (MG), creatinine (CTN), guanidinoacetic acid (GAA), guanidinobutyric acid (GBA), guanidinopropionic acid (GPA), argenine (Arg), and guanidinosuccinic acid (GSA), using isovaleroylacetone (IVA) and ethyl chloroformate (ECF) as derivatizing reagents. The separation was obtained from column HP-5 (30 m × 0.32 mm i.d.) with film thickness of 0.25 μm within 11 min. The linear calibrations were obtained with 0.5 to 50 μg/mL with coefficient of determination (R2) within 0.9969 – 0.9998. Limits of detections (LODs) were within 5 – 140 ng/mL. The derivatization, separation and determination was repeatable (n = 6) with relative standard deviation (RSD) within 1.2 – 3.1%. The guanidino compounds were determined in deproteinized serum of healthy volunteers and uremic patients within below LOD to 8.8 μg/mL and below LOD to 43.99 μg/mL with RSD within 1.4 – 3.6%. The recovery of guanidino compounds calculated by standard addition from serum was within 96.1 – 98.9%, with RSD 1.4 – 3.6%.

収録刊行物

  • Analytical Sciences

    Analytical Sciences 32 (2), 141-146, 2016

    社団法人 日本分析化学会

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