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Záver Pri úprave vzorky pôdy metódou disperzie matrice na tuhej fáze okrem špecifického chromatografického stpca pozostávajúceho zo vzorky pôdy homogenizovanej so sorbentom v pomere hmotností 1:1 sa na dno kolóny za sucha poklepkávaním plní vrstva sorbentu. Pomer hmotnosti sorbentu ku hmotnosti vzorky pôdy 1:1 vyplynul zo štúdia v práci [14]. V dôsledku toho získaný desorbát je íry a nie je potrebné ho pred odparením filtrova alebo centrifugova. Práca je zameraná na optimalizáciu extrakných parametrov a to objemu extrakného inidla, objemu zachytenej frakcie, objemu odparku, koneného objemu vzorky a prietokovej rýchlosti extrakného inidla. Pri MSPD sa na koncentranej úrovni 2,5 μg/g úinnosti extrakcie pohybovali pre prídavok zmesného štandardu do extraktu nekontaminovanej vzorky pôdy v rozmedzí 84-109 % a pre kontaminovanú pôdnu vzorku 62-94%. Detekné limity pesticídov sa pohybovali v rozmedzí 31- 87 ng/ml dávkovaného roztoku zmesi analytov. Práca vznikla za podpory projektov APVV-0597-07 , VVCE-0070-07, VEGA 1/0870/09. Literatúra [ 1] http://www.alanwood.net/pesticides , 13:00, 11.10.2008. [ 2] http://www.agrocourier.com/bayer/cropscience/cscms.nsf/id/Safener_ 10:00, 20.2.2009. [ 3] www.wikipedia.org , 10:00, 30.9.2008. [ 4] http://www.beyondpesticides.org/infoservices/pesticidefactsheets/toxic/pyrethroid.htm , 25.3.2005. [ 5] J. Garey, M. S. Wolf, Biochemical and Biophysical research communications 251, (1998) 855. [ 6] http://www.land.gov.sk/sk/index.php?navID=21&navID2=21&sID=23&id=385 , 16:00, 8.3.2009. [ 7] M. Kirchner, E. Matisova: Súasné metódy a nové trendy v izolácii reziduí pesticídov z beztukových potravín, Chem. Listy 98, (2004) 396405. [ 8] S.A. Barker, A.R. Long, in: V.K. Agarwal (Ed.), Analysis of Antibiotic Drug Residues in Food Products of Animal Origin, Plenum Press, New York, (1992) 119. [ 9] S.A. Barker, LC-GC Int. 11 (1998) 719. [10] Steven A. Barker.: Matrix solid-phase dispersion, Journal of Chromatography A, 885, (2000) 115-127. [11] G. Karasová, E. Brandšteterová, M. Lachová, Czech J. Food Sci. Vol. 21 (2003) 219. [12] S.A. Barker, Chemtech 23 (1993) 42. [13]. S.A. Barker, Z.E. Floyd, in: J. Pesek, M. Matyska, R. Abuelafiya (Eds.), Chemically Modified Surfaces: Recent Developments, Royal Society of Chemistry, (1996) 66. [14] Z. Michaloviová, Diplomová práca, Prif UK Bratislava (2005). Zborník príspevkov z 18. medzinárodnej vedeckej konferencie "Analytické metódy a zdravie loveka", ISBN 978-80-969435-7-9 - 115 - hotel Falkensteiner, Bratislava 11. - 14. 10. 2010

SIMULTANOUS DETERMINATION OF GALACTITOL AND GALACTOSE IN AQUEOUS SAMPLES BY GAS CHROMATOGRAPHY – MASS SPECTROMETRY IVAN OSTROVSKÝ*, RÓBERT KUBINEC, JAROSLAV BLAŠKO, JOZEF VIŠOVSKÝ, RENÁTA GÓROVÁ, GABRIELA ADDOVÁ, PETER PODOLEC, ALEXANDRA SZABÓOVÁ Chemical Institute, Faculty of Natural Sciences, Comenius University, Mlynská dolina CH-2, SK-845 45 Bratislava, Slovakia e-mail: ostrovsky@rec.uniba.sk Abstract Galactosemia, a metabolic disorder associated with the intolerance of dietary galactose due to an inherited enzymatic deficiency, is indicated by heightened levels of galactose and galactitol in urine. Gas chromatography (GC) with mass spectrometry (MS) detection was evaluated for its ability to screen urinary carbohydrates, particularly galactose and galactitol. The described method uses trimethylsilyl derivates of galactitol and galactose, and needs 100 l of urine for a single run. Spontaneous urine was obtained from 25 healthy subjects (classified into 5 age groups), from 4 treated patients with classical galactosaemia. The age dependences of galactose and galactitol excretion in urine was found in healthy subjects and treated galactosaemic patients by using reported method. Recognizing the clinical need for the simultaneous measurement of galactitol and galactose in urine for galactosaemic subjects, we developed the new GC/MS method, permits for the first time, measurement in urine by an accurate and precise single step procedure. This method does not require urine pretreatment before the silylation. Introduction Metabolism is the sum of all continuous biochemical reactions of breakdown and renewal of tissues of the body. Enzymes play an indispensable role in facilitating the process by serving as catalysts in the conversion of one chemical (metabolite) to another, often extracting the energy required for the reaction from a suitable high energy source, such as ATP [1]. Figure 1 shows the various possible mutation–sensitive defects affecting the compartmentalization and metabolism of compound A. This figure shows schematically the relationship between various defect types and their pathophysiologically and diagnostically important consequences [1]. Membrane 1 2 Holoenzyme Aoutside Ainside B C E 6 Fig. 1. The primary consequences of inborn errors of metabolism. 1–transporter-mediated movement of A from one compartment to another, 2–defect in the conversion of B to C, 3–increased conversion of B to D caused by accumulation of B, 4–defect in the interaction between an apoenzyme and an obligatory cofactor, 5–decreased feedback inhibition of the conversion of Ain to B as a result of deficiency of C, 6–secondary inhibition of the conversion of E to F caused by accumulation of D [1]. D 5 - F 4 Apoenzyme + cofactor “Inborn metabolic diseases” (IMDs) is the term applied to genetic disorders caused by loss of function of an enzyme. Enzyme activity may be low or lacking for variety of reasons. Some IMDs produce relatively unimportant physical features or skeletal abnormalities, but others produce serious diseases and even death. Most inborn errors of metabolism are monitored by blood or urine tests [2]. The phrase “inborn errors of metabolism” had been first used by A. E. Garrod in the Croonian Lectures of 1908, and published as a monograph with this title in 1909 [3]. Traditionally the IMDs are categorized as disorders of carbohydrate metabolism, amino acid metabolism, organic acid metabolism, or lysosomal storage diseases [4]. Galactosemia was first "discovered" in 1908, when Von Ruess reported on a breast-fed infant with failure to thrive, enlargement of the liver and spleen, and "galactosuria" in publication entitled "Sugar Excretion in Infancy". This infant ceased to excrete galactose through urine when milk products were removed from the diet. The toxic syndrome, galactosemia, is associated with an intolerance to dietary galactose as a result of certain enzymatic deficiencies [5]. Malfuctions in the following three enzymes, which participate in the normal metabolism of galactose (Fig. 2), are known to be causes of galactosemia: galactose-1-phosphate uridyltransferase (GALT), galactokinase and uridine diphosphate- Zborník príspevkov z 18. medzinárodnej vedeckej konferencie "Analytické metódy a zdravie loveka", ISBN 978-80-969435-7-9 - 116 - hotel Falkensteiner, Bratislava 11. - 14. 10. 2010

Záver<br />

Pri úprave vzorky pôdy metódou disperzie matrice na tuhej fáze okrem špecifického chromatografického stpca<br />

pozostávajúceho zo vzorky pôdy homogenizovanej so sorbentom v pomere hmotností 1:1 sa na dno kolóny za sucha<br />

poklepkávaním plní vrstva sorbentu. Pomer hmotnosti sorbentu ku hmotnosti vzorky pôdy 1:1 vyplynul zo štúdia v práci<br />

[14]. V dôsledku toho získaný desorbát je íry a nie je potrebné ho pred odparením filtrova alebo centrifugova. Práca je<br />

zameraná na optimalizáciu extrakných parametrov a to objemu extrakného inidla, objemu zachytenej frakcie, objemu<br />

odparku, koneného objemu vzorky a prietokovej rýchlosti extrakného inidla. Pri MSPD sa na koncentranej úrovni 2,5<br />

μg/g úinnosti extrakcie pohybovali pre prídavok zmesného štandardu do extraktu nekontaminovanej vzorky pôdy v<br />

rozmedzí 84-109 % a pre kontaminovanú pôdnu vzorku 62-94%. Detekné limity pesticídov sa pohybovali v rozmedzí 31-<br />

87 ng/ml dávkovaného roztoku zmesi analytov.<br />

Práca vznikla za podpory projektov APVV-0597-07 , VVCE-0070-07, VEGA 1/0870/09.<br />

Literatúra<br />

[ 1] http://www.alanwood.net/pesticides , 13:00, 11.10.2008.<br />

[ 2] http://www.agrocourier.com/bayer/cropscience/cscms.nsf/id/Safener_ 10:00, 20.2.2009.<br />

[ 3] www.wikipedia.org , 10:00, 30.9.2008.<br />

[ 4] http://www.beyondpesticides.org/infoservices/pesticidefactsheets/toxic/pyrethroid.htm , 25.3.2005.<br />

[ 5] J. Garey, M. S. Wolf, Biochemical and Biophysical research communications 251, (1998) 855.<br />

[ 6] http://www.land.gov.sk/sk/index.php?navID=21&navID2=21&sID=23&id=385 , 16:00, 8.3.2009.<br />

[ 7] M. Kirchner, E. Matisova: Súasné metódy a nové trendy v izolácii reziduí pesticídov z beztukových potravín, Chem.<br />

Listy 98, (2004) 396405.<br />

[ 8] S.A. Barker, A.R. Long, in: V.K. Agarwal (Ed.), Analysis <strong>of</strong> Antibiotic Drug Residues in Food Products <strong>of</strong> Animal<br />

Origin, Plenum Press, New York, (1992) 119.<br />

[ 9] S.A. Barker, LC-GC Int. 11 (1998) 719.<br />

[10] Steven A. Barker.: Matrix solid-phase dispersion, Journal <strong>of</strong> Chromatography A, 885, (2000) 115-127.<br />

[11] G. Karasová, E. Brandšteterová, M. Lachová, Czech J. Food Sci. Vol. 21 (2003) 219.<br />

[12] S.A. Barker, Chemtech 23 (1993) 42.<br />

[13]. S.A. Barker, Z.E. Floyd, in: J. Pesek, M. Matyska, R. Abuelafiya (Eds.), Chemically Modified Surfaces: Recent<br />

Developments, Royal Society <strong>of</strong> Chemistry, (1996) 66.<br />

[14] Z. Michaloviová, Diplomová práca, Prif UK Bratislava (2005).<br />

<strong>Zborník</strong> <strong>príspevkov</strong><br />

z 18. medzinárodnej <strong>vedeckej</strong> <strong>konferencie</strong><br />

"Analytické metódy a zdravie loveka", ISBN 978-80-969435-7-9<br />

- 115 -<br />

hotel Falkensteiner, Bratislava<br />

11. - 14. 10. 2010

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