A high-performance liquid chromatographic method for the determination of polyamines in milk is described. Polyamines were extracted in perchloric acid and derivatized with 9-fluorenylmethoxycarbonyl chloride (FMOC-Cl). The excess of reagent was reacted with aspartic acid before the analysis on a column-switching system. Linearity of derivatization was calculated for each amine and the coefficient of regression ranged from 0.994 to 0.999. Chromatographic separation of FMOC-polyamines was achieved with a gradient elution programme of water-acetonitrile. The correlation coefficients of the standard curves in the concentration range from 0.5 to 5 nmol ml(-1) were higher than 0.991. The repeatability of the method, expressed as R.S.D. for each polyamines ranged from 3.0 to 8.6%. The percent mean recoveries at 1 nmol ml(-1) spiking level were 49+/-3, 58+/-5, 61+/-5 and 48+/-4 for putrescine, cadaverine, spermidine and spermine, respectively. The limit of detection, calculated on the basis of three times signal-to-noise ratio, was 50 pmol ml(-1) for each polyamine

High-performance liquid chromatographic determination of polyamines in milk as their 9-fluorenylmethoxycarbonyl derivatives using a column-switching technique / F. Bellagamba, T. Mentasti, A. Albertini, U. Luzzana, V.M. Moretti, F. Valfrè. - In: JOURNAL OF CHROMATOGRAPHY A. - ISSN 0021-9673. - 791:1/2(1997), pp. 79-84.

High-performance liquid chromatographic determination of polyamines in milk as their 9-fluorenylmethoxycarbonyl derivatives using a column-switching technique

F. Bellagamba
Primo
;
T. Mentasti;V.M. Moretti
Penultimo
;
F. Valfrè
Ultimo
1997

Abstract

A high-performance liquid chromatographic method for the determination of polyamines in milk is described. Polyamines were extracted in perchloric acid and derivatized with 9-fluorenylmethoxycarbonyl chloride (FMOC-Cl). The excess of reagent was reacted with aspartic acid before the analysis on a column-switching system. Linearity of derivatization was calculated for each amine and the coefficient of regression ranged from 0.994 to 0.999. Chromatographic separation of FMOC-polyamines was achieved with a gradient elution programme of water-acetonitrile. The correlation coefficients of the standard curves in the concentration range from 0.5 to 5 nmol ml(-1) were higher than 0.991. The repeatability of the method, expressed as R.S.D. for each polyamines ranged from 3.0 to 8.6%. The percent mean recoveries at 1 nmol ml(-1) spiking level were 49+/-3, 58+/-5, 61+/-5 and 48+/-4 for putrescine, cadaverine, spermidine and spermine, respectively. The limit of detection, calculated on the basis of three times signal-to-noise ratio, was 50 pmol ml(-1) for each polyamine
derivatization, LC ; polyamines ; putrescine ; spermidine ; spermine
Settore AGR/19 - Zootecnica Speciale
http://www.sciencedirect.com/science/article/pii/S0021967397008066
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Utilizza questo identificativo per citare o creare un link a questo documento: http://hdl.handle.net/2434/65118
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