The Merrifield peptide synthesis studied by near-infrared Fourier-transform Raman spectroscopy

Larsen, Bjarne Due; Christensen, D. H.; Holm, Arne; Zillmer, R.; Nielsen, O. Faurskov

doi:10.1021/ja00067a044

Cited by 54 publications

(47 citation statements)

References 4 publications

(4 reference statements)

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“…Shrinkage temperature can easily be measured using thermal microscopy, using only a small amount of a sample [10]. The higher the shrinkage temperature, the better is the condition of the parchment object [9][10][11][12][13].…”

Section: The Influence Of Lipids On Parchment Degradationmentioning

confidence: 99%

“…However, studies of historic materials are difficult due to unknown storage history, production methods and inhomogeneous composition and structure [7], and techniques from macro to nanoscale may be necessary [8]. Shrinkage temperature has been reported to be a good indicator of hydrothermal stability, and indicative of the level of deterioration of collagen fibres [9,10]. The higher the shrinkage temperature, the more energy is needed for bonds to break between collagen molecules, thus indicating better condition of the parchment object [9][10][11][12][13].…”

Section: Introductionmentioning

confidence: 99%

“…Shrinkage temperature has been reported to be a good indicator of hydrothermal stability, and indicative of the level of deterioration of collagen fibres [9,10]. The higher the shrinkage temperature, the more energy is needed for bonds to break between collagen molecules, thus indicating better condition of the parchment object [9][10][11][12][13]. Other thermal methods to study the condition of parchment have been suggested [6,[11][12][13][14], one of the most commonly used methods being differential scanning calorimetry (DSC) [9,15].…”

Section: Introductionmentioning

confidence: 99%

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On oxidative degradation of parchment and its non-destructive characterisation and dating

Možir

Strlič²,

Trafela

et al. 2010

Appl. Phys. A

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Historic parchment is an extremely complex material, not only due to the various methods of production used and various past environmental histories of objects, but also due to its inhomogeneous structure. Many traditional methods of characterisation are empirical, but useful since they have gained recognition by the end-users. In this paper, we investigated the shrinkage temperature of collagen and the influence of lipids contained in parchment on the measurements. While the content of lipids does not seem to significantly affect shrinkage temperature measurements themselves, it strongly affects the decrease of shrinkage temperature of collagen during degradation, and thus its thermomechanical properties. This confirms the high importance of lipid peroxidation during degradation of parchment.While shrinkage temperature determination is a micro-destructive method, we also demonstrated that it is possible to determine this property using near infrared (NIR) spectroscopy based on partial least squares calibration. The root-mean square error of validation (RMSEV), obtained on a set of variously delipidised and degraded samples, was 7 o C, so the method could be used for condition assessment or classification of historic objects. Using a set of 185 historic objects dating from 1200-1800, we also developed a method for non-destructive dating of parchment based on NIR spectroscopy using partial least squares calibration (RMSEV = 72 years), and successfully determined the correct age of a historic charter from the collection of Nationaal Archief, The Netherlands.

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Section: The Influence Of Lipids On Parchment Degradationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

On oxidative degradation of parchment and its non-destructive characterisation and dating

Možir

Strlič²,

Trafela

et al. 2010

Appl. Phys. A

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“…The main consequence is that solid-phase reactions are often left to run for longer than necessary (to ensure a complete reaction). Some methods have been employed in SPOS such as NMR gelphase spectroscopy or magic angle NMR spectroscopy, [2][3][4][5][6] fluorescence spectroscopy, 7 and Fourier Transform Infrared Spectroscopy (FT-IR) including Raman FT-IR, 8,9 Attenuated Total Reflection 10 and FT-IR microspectroscopy 11 and KBr pellets by Infrared difference spectra. 12 Though invaluable, these techniques require instrumentation that is often prohibitively expensive.…”

Section: Introductionmentioning

confidence: 99%

An efficient monitoring technique for solid-phase reactions by KBr pellets/FT-IR using methyl p-aminobenzoate synthesis assisted by microwave radiation on merrifield resin

Antonow¹,

Graebin²,

Eifler‐Lima³

2004

J. Braz. Chem. Soc.

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O uso de pastilhas de KBr em espectroscopia de infravermelho foi investigado para a monitorização de reações em fase sólida. A síntese do p-aminobenzoato de metila na Resina Merrifield (RM) é descrita como um modelo para esta técnica, a qual permite que o progresso das três etapas da síntese sejam monitoradas.The use of KBr pellets in infrared spectroscopy has been investigated for monitoring solidphase reactions. Synthesis of the methyl p-aminobenzoate on Merrifield resin (MR) is described as a model for this technique, which allows the progress of its three on-bead reaction steps to be monitored throughout their duration.

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“…It was shown that the cleavage of the Fmoc protecting group was related to the secondary structure of the resin-bound peptide. 15,16 In particular,ˇ-sheet formation caused problems.…”

Section: Introductionmentioning

confidence: 99%

Secondary structure and association of melittin during and after solid‐phase synthesis: a Raman and static light scattering study

Hansen

Callisen

et al. 2002

J Raman Spectroscopy

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The solid-phase synthesis of melittin, a haemolytic peptide containing 26 amino acid residues, was monitored by near-infrared Fourier transform Raman spectroscopy. The resin used was Tenta Gel S RAM. The secondary peptide structure was investigated for each step in the synthesis. A random coil secondary structure was the most probable in all cases, and accordingly all steps in the synthesis gave good yields. Melittin cleaved from the resin showed an a-helix secondary structure in the solid state. Raman spectra were obtained for 10, 5, 4, 2 and 1% (w/w) aqueous solutions. The 1 and 2% solutions showed too weak melittin bands to be able to draw conclusions about the secondary structure. However, the more concentrated solutions evidently showed an a-helical structure. Simultaneous static light scattering, refractive index measurements and exclusion chromatography on synthetic melittin in 50 mM phosphate (pH 7) and 150 mM NaCl showed the presence of dimers and tetramers in the eluted liquid. No evidence of monomers or trimers was found.

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The Merrifield peptide synthesis studied by near-infrared Fourier-transform Raman spectroscopy

Cited by 54 publications

References 4 publications

On oxidative degradation of parchment and its non-destructive characterisation and dating

On oxidative degradation of parchment and its non-destructive characterisation and dating

An efficient monitoring technique for solid-phase reactions by KBr pellets/FT-IR using methyl p-aminobenzoate synthesis assisted by microwave radiation on merrifield resin

Secondary structure and association of melittin during and after solid‐phase synthesis: a Raman and static light scattering study

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