Higher Order Inclusion Complexes and Secondary Interactions Studied by Global Analysis of Calorimetric Titrations

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Resumé

This paper investigates the use of isothermal titration calorimetry (ITC) as a tool for studying molecular systems in which weaker secondary interactions are present in addition to a dominant primary interaction. Such systems are challenging since the signal pertaining to the stronger primary interaction tends to overshadow the signal from the secondary interaction. The methodology presented here enables a complete and precise thermodynamic characterization of both the primary and the weaker secondary interaction, exemplified by the binding of β-cyclodextrin to the primary and secondary binding sites of the bile salt glycodeoxycholate. Global regression analysis of calorimetric experiments at various concentrations and temperatures provide a precise determination of ΔH, ΔG°, and ΔCp for both binding sites in glycodeoxycholate (K1 = 5.67 ± 0.05 × 103 M–1, K2 = 0.31 ± 0.02 × 103 M–1). The results are validated by a 13C NMR titration and negative controls with a bile salt with no secondary binding site (glycocholate) (K = 2.96 ± 0.01 × 103 M–1). The method proved useful for detailed analysis of ITC data and may strengthen its use as a tool for studying molecular systems by advanced binding models.

OriginalsprogEngelsk
TidsskriftAnalytical Chemistry
Vol/bind84
Udgave nummer5
Sider (fra-til)2305-2312
ISSN0003-2700
DOI
StatusUdgivet - 2012

Citer dette

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title = "Higher Order Inclusion Complexes and Secondary Interactions Studied by Global Analysis of Calorimetric Titrations",
abstract = "This paper investigates the use of isothermal titration calorimetry (ITC) as a tool for studying molecular systems in which weaker secondary interactions are present in addition to a dominant primary interaction. Such systems are challenging since the signal pertaining to the stronger primary interaction tends to overshadow the signal from the secondary interaction. The methodology presented here enables a complete and precise thermodynamic characterization of both the primary and the weaker secondary interaction, exemplified by the binding of β-cyclodextrin to the primary and secondary binding sites of the bile salt glycodeoxycholate. Global regression analysis of calorimetric experiments at various concentrations and temperatures provide a precise determination of ΔH, ΔG°, and ΔCp for both binding sites in glycodeoxycholate (K1 = 5.67 ± 0.05 × 103 M–1, K2 = 0.31 ± 0.02 × 103 M–1). The results are validated by a 13C NMR titration and negative controls with a bile salt with no secondary binding site (glycocholate) (K = 2.96 ± 0.01 × 103 M–1). The method proved useful for detailed analysis of ITC data and may strengthen its use as a tool for studying molecular systems by advanced binding models.",
author = "Sch{\"o}nbeck, {Jens Christian Sidney} and Ren{\'e} Holm and Peter Westh",
year = "2012",
doi = "10.1021/ac202842s",
language = "English",
volume = "84",
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journal = "Analytical Chemistry",
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Higher Order Inclusion Complexes and Secondary Interactions Studied by Global Analysis of Calorimetric Titrations. / Schönbeck, Jens Christian Sidney; Holm, René; Westh, Peter.

I: Analytical Chemistry, Bind 84, Nr. 5, 2012, s. 2305-2312.

Publikation: Bidrag til tidsskriftTidsskriftartikelForskningpeer review

TY - JOUR

T1 - Higher Order Inclusion Complexes and Secondary Interactions Studied by Global Analysis of Calorimetric Titrations

AU - Schönbeck, Jens Christian Sidney

AU - Holm, René

AU - Westh, Peter

PY - 2012

Y1 - 2012

N2 - This paper investigates the use of isothermal titration calorimetry (ITC) as a tool for studying molecular systems in which weaker secondary interactions are present in addition to a dominant primary interaction. Such systems are challenging since the signal pertaining to the stronger primary interaction tends to overshadow the signal from the secondary interaction. The methodology presented here enables a complete and precise thermodynamic characterization of both the primary and the weaker secondary interaction, exemplified by the binding of β-cyclodextrin to the primary and secondary binding sites of the bile salt glycodeoxycholate. Global regression analysis of calorimetric experiments at various concentrations and temperatures provide a precise determination of ΔH, ΔG°, and ΔCp for both binding sites in glycodeoxycholate (K1 = 5.67 ± 0.05 × 103 M–1, K2 = 0.31 ± 0.02 × 103 M–1). The results are validated by a 13C NMR titration and negative controls with a bile salt with no secondary binding site (glycocholate) (K = 2.96 ± 0.01 × 103 M–1). The method proved useful for detailed analysis of ITC data and may strengthen its use as a tool for studying molecular systems by advanced binding models.

AB - This paper investigates the use of isothermal titration calorimetry (ITC) as a tool for studying molecular systems in which weaker secondary interactions are present in addition to a dominant primary interaction. Such systems are challenging since the signal pertaining to the stronger primary interaction tends to overshadow the signal from the secondary interaction. The methodology presented here enables a complete and precise thermodynamic characterization of both the primary and the weaker secondary interaction, exemplified by the binding of β-cyclodextrin to the primary and secondary binding sites of the bile salt glycodeoxycholate. Global regression analysis of calorimetric experiments at various concentrations and temperatures provide a precise determination of ΔH, ΔG°, and ΔCp for both binding sites in glycodeoxycholate (K1 = 5.67 ± 0.05 × 103 M–1, K2 = 0.31 ± 0.02 × 103 M–1). The results are validated by a 13C NMR titration and negative controls with a bile salt with no secondary binding site (glycocholate) (K = 2.96 ± 0.01 × 103 M–1). The method proved useful for detailed analysis of ITC data and may strengthen its use as a tool for studying molecular systems by advanced binding models.

U2 - 10.1021/ac202842s

DO - 10.1021/ac202842s

M3 - Journal article

VL - 84

SP - 2305

EP - 2312

JO - Analytical Chemistry

JF - Analytical Chemistry

SN - 0003-2700

IS - 5

ER -