Amniyotik Sıvıda Süksinilasetonun Elektrokimyasal Davranışı Ve Tayini

Öz

Süksinilaseton (SA, 4,6 diketoheptanoik asit), kalıtsal hepatorenal tirozinemi tip I hastalığı için birincil tanı metabolitidir. Bu çalışma ile süksinilasetonun amniyon sıvısında voltametrik tayinini amaçlanmıştır. Voltametri için optimum koşullar belirlenmiştir. Destek elektrolit için 0,10 mol/L potasyum klorür kullanılmıştır. Çalışmada, asılı civa damlası (HMDE) çalışma elektrotu olarak seçilirken, referans elektrot Ag/AgCl (3M KCI), karşıt elektrot Pt olarak kullanılmıştır. Kalibrasyon için kare dalga voltametri kullanılmış, bu yöntem amniyotik sıvıya uygulandığında, süksinilaseton ekstraksiyon işleminin, metil ester oluşturduğu tespit edilmiştir. Süksinilaseton metil esteri, yapısal olarak süksinilasetondan farklı olduğu için elektrokimyasal davranışı tekrar çalışılmıştır. Voltametrik inceleme, süksinilaseton metil esterinin iki elektron transferi ile indirgendiğini göstermiştir. Doğrusallık aralığı 5,83xE-05 – 3,25xE-06 mol/L derişimleri arasındadır. Tespit limiti (LOD) ve tayin limiti (LOQ) sırasıyla 2,72xE-07 mol/L ve 9,08xE-07 mol/L olarak hesaplanmıştır. Amniyotik sıvı içindeki süksinilaseton metil esteri kare dalga voltametri ile analiz edilmiştir. Geri alınabilirlik %88,1 bulunmuştur.

Anahtar Kelimeler

• Süksinilaseton
• Süksinilaseton metil ester
• Voltametri

Electrochemical Behavior and Determination of Succinylacetone in Amniotic Fluid

Öz

Succinylacetone (SA, 4,6 diketoheptanoic acid) is the primare diagnosis metabolite for hereditable hepatorenal tyrosinemia type I disease. In present researh, voltammetric analysis of succinylacetone was aimed. The optimum conditions for voltammetry were determined. Optimum conditions for voltammetry were determined. Potassium chloride 0.10 mol/L was selected for the support electrolyte. For the experiments, hanging mercury drop (HMDE), Ag/AgCl (3M KCI) reference and Pt counter electrodes were used. Square wave voltammetry was used for calibration and when this method was applied to amniotic fluid, succinylacetone extraction process was found to form methyl ester. Since succinylacetone methyl ester has a different structure than succinylacetone, its electrochemical behavior was re-examined. Voltammetric data reveal that succinylacetone methyl ester is reduced by accepting two electrons. For calibration, concentrations in the range of 3.25xE-06 mol/L – 5.83xE-05 mol/L were used. From the calibration chart, the limit of detection (LOD) was found to be 2.72xE-07 mol/L and the limit of determination (LOQ) was 9.08xE-07 mol/L. Succinylacetone methyl ester in amniotic fluid was analyzed by square wave voltammetry. The recoverability was found to be 88.1%.

Anahtar Kelimeler

• Succinylacetone
• Succinylacetone methyl ester
• Voltammetry

Kaynakça

1. Anonim. 2010. Prenantal Diagnosis. URL: http://www.genetikbilimi.com/genbilim/prenantal.htm (Erişim tarihi: 15 Haziran 2010).
2. Bond AM. 1980. Modern Polarographic Methods in Analytical Chemistry. Marcel Dekker, New York, USA, pp: 196.
3. Cansever MŞ, Erim FB. 2005. Determination of urinary succinyacetone by capillary elecrophoresis for the diagnosis of tyrosinemia type I. J Chromatogr B, 818: 309-311.
4. Cerda B, Cherkasskiy A, Li Y. 2008. United States Patent Application Publication. Pub. No. US2008/0274563 A1.
5. Cry D, Giguére R, Vilain, LB, Drouin R. 2006. A GC/MS validated method for the nanomolar range determination of succinyacetone in amniotic fluid and plasma: An analytical tool for tyrosinemia type I. J Chromatogr B, 832: 24-29.
6. Ermer J, Miller JHM. 2005. Method validation in pharmaceutical analysis: A guide to best practice. In: Ermer J, Miller JHM editors. Wiley, VCH Verlag GmbH & Co. KGaA, Weinheim, Germany, pp: 200.
7. Macsai MS, Schwartz TL, Hinkle D, Hummel MB, Mulhern MG, Rootman D. 2001. Tyrosinemia Type II: Nine Cases of Ocular Signs and Symptoms. Am J Ophthalmol, 132: 522-527.
8. Michael HG, Khaja B, Alberto B, Hsiao-Jan C, Yin-Hsiu C, George D, Christine D, Roberto G, Amy H, Xinying H, Shu-Min K, Hamid K, Tracy K, Francyne K, Hsuan-Chieh L, Monica M, Adrienne M, Joseph O, Yin P, Enzo R, Andreas R, Nicolas SF, Coleman TT, Frédérick MV, Li-yun W, and Dietrich M. 2022. Liquid Chromatography–Tandem Mass Spectrometry in Newborn Screening Laboratories. Int J Neonatal Screen. 8,4: 62.

9. Shinka T, Ohse M, Inoue Y, Kuhara T. 2005. Stability of 5-aminoevulinic acid on dried urine filter paper for a dignostic marker of tyrosinemia type I. J Chromatogr B, 823: 44–46.
10. Tuma P, Samcova E, Andelova K. 2006. Determination of free amino acids and related compounds in amniotic fluid by capillary electrophoresis with contactless conductivity detection. J Chromatogr B, 839:12-18.
11. Uslu B, Ozkan SA. 2004. Anodic voltammetry of abacavir and its determination in pharmaceuticals and biological fluids Electrochim Acta, 49(25): 4321–4329.
12. Wang J, Tuzhi P, Lin MS and Tapia T. 1986. Trace measurements of the antineoplastic agent methotrexate by adsorptive stripping voltammetry. Talanta, 33 (9): 707-712.