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The guanidino compounds guanidine, methylguanidine, guanidinoacetic acid, guanidinopropionic acid, guanidinobutyric acid and guanidinosuccinic acid were eluted and separated after pre-column derivatization with glyoxal from an HP-5 column (30 m × 0.32 mm i.d.) with film thickness 0.25 µm at an initial column temperature of 100°C for 2 min, with ramping of 20°C/min up to 250°C and a nitrogen flow rate of 3 mL/min. Detection was by flame ionization detection. Linear calibrations were observed within 0.1–20.0 µmol/L, with limit of detection within 0.024–0.034 µmol/L for each compound. The separation was repeatable with relative standard deviation (RSD) ( n  = 6) within 1.2–1.8 and 1.1–1.6% in terms of retention time and peak height/peak area, respectively. The method was applied for the determination of the guanidino compounds from serum of uremic patients ( n  = 7) and healthy volunteers ( n  = 8), and amounts were observed within 1.33–11.71 and 0.07–0.39 µmol/L with RSD 1.1–3.5 and 1.1–3.0%, respectively. The results were further supported by the standard addition method.

Gas Chromatographic Determination of Guanidino Compounds in Uremic Patients Using Glyoxal as Derivatizing Reagent