Analytical Sciences
Online ISSN : 1348-2246
Print ISSN : 0910-6340
ISSN-L : 0910-6340
Original Papers
Improved Gas Chromatographic Determination of Guanidino Compounds Using Isovaleroylacetone and Ethyl Chloroformate as Derivatizing Reagents
Rizwan Ali ZOUNRMumammad Yar KHUHAWARTaj Muhammad JAHANGIRMalik ALAMGIR
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2016 Volume 32 Issue 2 Pages 141-146

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Abstract

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%.

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© 2016 by The Japan Society for Analytical Chemistry
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