Gas Chromatographic Analysis of Guanidino Compounds in Sera and Urine of Uremic Patients Using Glyoxal and Ethyl Chloroformate as Derivatizing Reagents

作者：Majidano Subhan Ali^*; Khuhawar Muhammad Yar

来源：Analytical Sciences, 2013, 29(2): 221-226.

Gas chromatographic (GC) method has been developed for the determination of the guanidino compounds: guanidine (G), methylguanidine (MG), guanidinoacetic acid (GAA), guanidinopropionic acid (GPA), guanidinobutyric acid (GBA) and guanidinosuccinic acid (GSA) was carried out after precolumn derivatization with glyoxal and ethyl chloroformate from the column HP-5 (30 m x 0.32 min i.d.) at 90 degrees C for 3 min, followed by a heating rate 25 degrees C/min up to 260 degrees C with a nitrogen flow rate of 2 ml/min. Detection was by FID. The linear calibrations were obtained within 0.1 - 20.0 mu mol/L, with limits of detection (LODs) within 0.014 - 0.024 mu mol/L. The separation and derivatization was repeatable (n = 6) with relative standard deviations (RSD) within 0.8 - 1.9% in retention time and 0.5 - 1.8% in peak height/peak area. A number of additives and amino acids did not affect the determination. The method was applied for the determination of guanidino compounds from the serum and urine of 9 healthy volunteers and 8 uremic patients and the amounts found were in the range 0.08 - 0.48 and below the limit of detection (LOD) - 345 mu mol/L and 1.82 - 13.88 and 0.77 - 432.0 mu mol/L with RSDs within 4.2%, respectively.

• 出版日期2013-2