GC-MS analysis of monosaccharide mixtures as their diethyldithioacetal derivatives: Application to plant gums used in art works

Pitthard, Václav; Finch, Paul

doi:10.1007/bf02490349

Cited by 50 publications

(27 citation statements)

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“…Moreover the analysis of saccharide materials in paint samples needs an additional step of purification, in order to remove pigments and fillers. There are many different chemolysis procedures used to study plant gums [6], based on: the methanolysis [7,8], on the hydrolysis [9-13], and hydrolysis assisted by microwaves of the polysaccharide [14-16]. Rates of degradation differ for each monosaccharide during hydrolysis.…”

Section: Introductionmentioning

confidence: 99%

“…It is very difficult to analyze all three types of sugars in one quantitative analysis without creating multiple derivatives of each sugar [23]. To avoid the formation of multiple derivatives, which occur because sugars have different isomeric forms in solution [24], various derivatisation procedures have been proposed, such as the reduction of carbonyl moieties followed by acetylation [25,26] the conversion of monosaccharides into acyclic oximes, followed by silylation [11] or acetylation [9,10], or the formation of diethyl mercaptal derivatives followed by silylation [13,27]. Each of these methodologies has its own advantages and drawbacks [1], but none of them is able to derivatise aldoses, ketoses and uronic acids at the same time without inducing any degradation, or producing chromatograms too complex to be unequivocally interpreted.…”

Section: Introductionmentioning

confidence: 99%

“…Because of these inherent difficulties, those analyzing carbohydrates in the field of cultural heritage are not able to fully compare data obtained from a variety of different analytical methodologies, because each of them produce extremely different chromatographic profiles and multiple databases [13,28,29]. Moreover, in most cases the results of the quantitative analyses are not given, so that evaluating the sugar profiles of the paint samples are even more complex.…”

Section: Introductionmentioning

confidence: 99%

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Analysis of plant gums and saccharide materials in paint samples: comparison of GC-MS analytical procedures and databases

Lluveras‐Tenorio

Mazurek

Restivo

et al. 2012

Chemistry Central Journal

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BackgroundSaccharide materials have been used for centuries as binding media, to paint, write and illuminate manuscripts and to apply metallic leaf decorations. Although the technical literature often reports on the use of plant gums as binders, actually several other saccharide materials can be encountered in paint samples, not only as major binders, but also as additives. In the literature, there are a variety of analytical procedures that utilize GC-MS to characterize saccharide materials in paint samples, however the chromatographic profiles are often extremely different and it is impossible to compare them and reliably identify the paint binder.ResultsThis paper presents a comparison between two different analytical procedures based on GC-MS for the analysis of saccharide materials in works-of-art. The research presented here evaluates the influence of the analytical procedure used, and how it impacts the sugar profiles obtained from the analysis of paint samples that contain saccharide materials. The procedures have been developed, optimised and systematically used to characterise plant gums at the Getty Conservation Institute in Los Angeles, USA (GCI) and the Department of Chemistry and Industrial Chemistry of the University of Pisa, Italy (DCCI). The main steps of the analytical procedures and their optimisation are discussed.ConclusionsThe results presented highlight that the two methods give comparable sugar profiles, whether the samples analysed are simple raw materials, pigmented and unpigmented paint replicas, or paint samples collected from hundreds of centuries old polychrome art objects. A common database of sugar profiles of reference materials commonly found in paint samples was thus compiled. The database presents data also from those materials that only contain a minor saccharide fraction. This database highlights how many sources of saccharides can be found in a paint sample, representing an important step forward in the problem of identifying polysaccharide binders in paint samples.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Analysis of plant gums and saccharide materials in paint samples: comparison of GC-MS analytical procedures and databases

Lluveras‐Tenorio

Mazurek

Restivo

et al. 2012

Chemistry Central Journal

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“…Monosaccharides in hydrolysates are usually analyzed by gas chromatography with flame ionization detection (GC-FID) and gas chromatography with mass spectrometric detection (GC-MS) (Koivula and Hänninen 2001;Pitthard and Finch 2001). High performance liquid chromatography (HPLC) and capillary electrophoresis (CE) are commonly used to separate monosaccharides (Lv et al 2009;Guttman 1997;Dahlman et al 2000), of which uronic acid is a derivative.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Separation and Quantitative Determination of Monosaccharides, Uronic Acids, and Aldonic Acids by High Performance Anion-Exchange Chromatography Coupled With Pulsed Amperometric Detection in Corn Stover Prehydrolysates

Wang¹,

Xu²,

Li³

et al. 2012

BioResources

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A method for simultaneous separation and quantitative determination of arabinose, galactose, glucose, xylose, xylonic acid, gluconic acid, galacturonic acid, and glucuronic acid was developed by using high performance anion-exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD). The separation was performed on a CarboPac TM PA-10 column (250 mm × 2 mm) with a various gradient elution of NaOH-NaOAc solution as the mobile phase. The calibration curves showed good linearity (R 2 ≥ 0.9993) for the monosaccharides, uronic acids, and aldonic acids in the range of 0.1 to 12.5 mg/L. The detection limits (LODs) and the quantification limits (LOQs) were 4.91 to 18.75 μg/L and 16.36 to 62.50 μg/L, respectively. Relative standard deviations (RSDs) of the retention times and peak areas for the seven consecutive determinations of an unknown amount of mixture were 0.15% to 0.44% and 0.22% to 2.31%, respectively. The established method was used to separate and determine four monosaccharides, two uronic acids, and two aldonic acids in the prehydrolysate from dilute acid steam-exploded corn stover within 21 min. The spiked recoveries of monosaccharides, uronic acids, and aldonic acids ranged from 91.25% to 108.81%, with RSDs (n=3) of 0.04% ~ 6.07%. This method was applied to evaluate the quantitative variation of sugar and sugar acid content in biomass prehydrolysates.

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“…GC/MS analysis of standard monosaccharides by the original derivatization method reported by Pitthard et al7) …”

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confidence: 99%

Analysis of Thickening Polysaccharides by the Improved Diethyldithioacetal Derivatization Method

Akiyama

Yamazaki²,

Tanamoto³

2011

Journal of the Food Hygienics Society of Japan

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The identification test for thickening polysaccharides containing neutral saccharides and uronic acids was investigated by GC analysis of constituent monosaccharides. The reported method, in which monosaccharides were converted to diethyldithioacetal derivatives with ethanethiol followed by trimethylsilylation, was improved in terms of operability and reproducibility of GC/MS analysis. The suitability of the improved diethyldithioacetal derivatization method was determined for seven thickening polysaccharides, i.e., carob bean gum, guar gum, karaya gum, gum arabic, gum ghatti, tragacanth gum and peach gum. The samples were acid-hydrolyzed to form monosaccharides. The hydrolysates were derivatized and analyzed with GC/FID. Each sugar derivative was detected as a single peak and was well separated from others on the chromatograms. The amounts of constituent monosaccharides in thickening polysaccharides were successfully estimated. Seven polysaccharides were distinguished from each other on the basis of constituent monosaccharides. Further examination of the time period of hydrolysis of polysaccharides using peach gum showed that the optimal times were not the same for all monosaccharides. A longer time was needed to hydrolyze glucuronic acid than neutral saccharides. The findings suggest that hydrolysis time may sometimes a#ect the analytical results on composition of constituent monosaccharides in polysaccharides.

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GC-MS analysis of monosaccharide mixtures as their diethyldithioacetal derivatives: Application to plant gums used in art works

Cited by 50 publications

References 12 publications

Analysis of plant gums and saccharide materials in paint samples: comparison of GC-MS analytical procedures and databases

Analysis of plant gums and saccharide materials in paint samples: comparison of GC-MS analytical procedures and databases

Simultaneous Separation and Quantitative Determination of Monosaccharides, Uronic Acids, and Aldonic Acids by High Performance Anion-Exchange Chromatography Coupled With Pulsed Amperometric Detection in Corn Stover Prehydrolysates

Analysis of Thickening Polysaccharides by the Improved Diethyldithioacetal Derivatization Method

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