0000000000970894
AUTHOR
R. Mateo Castro
Characterization of proteinaceous glues in old paintings by separation of the o-phtalaldehyde derivatives of their amino acids by liquid chromatography with fluorescence detection.
A HPLC-fluorescence method for characterization of proteinaceous glues from binding media used in pictorial works of art prior to conservation or restoration treatment is proposed. Fluorescence derivatization of amino acids released by acid hydrolysis of standard proteins is studied. The derivatization reagent was o-phtalaldehyde with 2-mercaptoethanol as catalyst. Mobile phase was a programmed gradient among two eluents (water buffered at pH 5.8 wit 5% THF, and methanol) and is able to satisfactorily resolve the amino acid derivatives in 45min. Peak area ratios among amino acid derivatives and the leucine derivative are useful to characterize the proteins. The method shows good sensitivity…
Characterization of waxes used in pictorial artworks according to their relative amount of fatty acids and hydrocarbons by gas chromatography.
A study attempted to characterize natural waxes used in pictorial works of art was carried out by means of gas chromatography. The analytical treatment requires prior hydrolysis of the waxes to release the fatty acids (FA) (myristic (myr), palmitic (pal), oleic (ole), stearic (ste), araquidic (ara), behenic (beh), lignoceric (lig), cerotic (cer)) from the main esters of the waxes. The formation of volatile derivatives of the fatty acids was carried out by derivatization with ethyl choroformate (ECF). This derivatization reagent was chosen due to the speed, safety and quantitativity of the reaction. The analyzed hydrocarbons were n-eicosane, n-heneicosane, n-docosane, n-tricosane, n-tetracos…
EVALUATION OF THE COLOR OF SOME SPANISH UNIFLORAL HONEY TYPES AS A CHARACTERIZATION PARAMETER
Abstract The color of 7 types of Spanish unifloral honey from rosemary, orange blossom, lavender, eucalyptus, sunflower, heather, and honeydew was Investigated for Its potential use as a characterization parameter. Colors were estimated by visual comparison with a Lovlbond 1000 Instrument, the readings of which were transformed Into Pfund units. As an alternative method, the transmittances of liquid samples at selected wavelengths were measured, trlstlmulus values were calculated, and chromatic coordinates In the CIE-1931 (x,y,L) and CIE-1976 (L*a*b*) color spaces were determined. The correlation coefficient between x and the Pfund grading was 0.958, but visual comparisons proved to be less…
Study of binding media in works of art by gas chromatographic analysis of amino acids and fatty acids derivatized with ethyl chloroformate
The aim of this work is to identify proteinaceous and oil binding media used in paintings from art collections in the Region of Valencia (Spain). This information is extremely useful for conservation and restoration work. The proposed procedure involves protein and glyceride hydrolysis from sub-milligram samples by treatment with hydrochloric acid, followed by neutralization, partition with chloroform and derivatization with ethyl chloroformate (ECF) of both the aqueous and the organic phases. The ECF derivatives of amino acids and azelaic, myristic, palmitic and stearic acids are separated by capillary gas chromatography. Amino acids are mainly found in the aqueous phase and long chain fat…
Identification of lipid binders in old oil paintings by separation of 4-bromomethyl-7-methoxycoumarin derivatives of fatty acids by liquid chromatography with fluorescence detection.
A HPLC-fluorescence method for identification of drying oils from binding media or protective film used in pictorial works of art prior to conservation or restoration is proposed. Fluorescence derivatization of fatty acids released by hydrolysis of structural drying oils is studied. The derivatization reagent was 4-(bromomethyl)-7-methoxycoumarin with 18-crown-6 as catalyst. Mobile phase was programmed from methanol-water (90:10 v/v) to methanol-water (100:0 v/v) in 25 min. The excitation and emission wavelengths were 325 and 395 nm, respectively. Under these chromatographic conditions, coumarin derivatives of myristic, palmitic, oleic and stearic acids were satisfactorily resolved. The met…
Identification of drying oils used in pictorial works of art by liquid chromatography of the 2-nitrophenylhydrazides derivatives of fatty acids.
A new HPLC-UV-Vis method for identification of drying oils from binding media or protective film used in pictorial works of art prior to conservation or restoration is proposed. Chromophore derivatization of fatty acids released by hydrolysis of structural drying oils is studied. The derivatization reagent selected was 2-nitrophenylhydrazine with 1-ethyl-3-(3-dimethyl animopropyl)carbodiimide hydrochloride/pyridine as catalyst. This reaction was carried out using microwave heating. Mobile phase was methanol/water/n-propanol/acetic acid (80:14:5:1) running in isocratic mode. Absorbance was measured at 400nm. In these conditions, hydrazides of myristic, palmitic, oleic, and stearic acids were…