Improved 19F{1H} Saturation Transfer Difference Experiments for Sensitive Detection to Fluorinated Compound Bound to Proteins

Kazuo Furihata,Mitsuru Tashiro

doi:10.3390/magnetochemistry5010001

Abstract

The 19F{1H} saturation transfer difference (STD) method was improved for sensitive 19F detection using a human serum albumin-diflunisal complex. Because NMR (nuclear magnetic resonance) experiments with 19F detection are feasible for the selective detection of fluorinated compounds, more sensitive NMR methods are required to be developed for purposes of practicality. The present research focused on the investigations of 19F{1H} STD pulse techniques and experimental parameters, leading to the development of detection methods with higher sensitivity.

Highlights

MInRtrod(nuuctciloenar magnetic resonance) spectroscopy can be a useful method for analyzing protein–ligand interactions in the solution state
Dwiefrleunisal optimized using the complex of diflunisal (Figure 1) and human serum albumin (HSA)
Diflunisal and HSA were purchased from Sigma-Aldrich (Tokyo, JaAplal nof).thAe 6N0M0-RμLspvecotlruamweeroefrseocolurdtieodnact o2n0t°aCinoinnga 0V.0ar5iamn M600HMSAHzaNndM2R.5symstMemdeiqfluuipnpiseadl was prepawreitdh ainn 1H0F0X%p2roHb2eO(V. arian, Palo Alto, CA, USA)

Summary

Introduction

MInRtrod(nuuctciloenar magnetic resonance) spectroscopy can be a useful method for analyzing protein–ligand interactions in the solution state. Various NMR-based screening methods to observNe M1HR (lniguaclnedar smigangnaelstichraevsoenbaenecen) sppreocptroossecdop, ysucacnhbaesaNusOefEu-lpmuemthpoidnfgor[1a]n,aslyaztiunrgaptiroonteitnra–nsfer ligand interactions in the solution state. Various NMR-based screening methods to observe dreivffeerr1[seH2en],lNcigewOaan(EtSde-Trps–Diulgim)gnaa[pnl2sid]nh, gaowv[be5as]ebtereevrex-enpldipegrravoinmipadoesgnoertdabsd,.ssieNuerncvMhteRadssp-bNevcaiOtasreEodg-spcrsouacpdmryeipeein(nnWtignas[g1tpe]mer, LcseatOrttuhoGrsoSacdYtois)opnhy[3atr,v(4aWe]n, saafaltesnerodrdLbirfOefeeevGrneeSrnasYcpee)p(N[lSi3OTe,d4DE]-)t,oa1n9dF detecptiuomnp[i6n–g9[]5. Dwiefrleunisal optimized using the complex of diflunisal (Figure 1) and human serum albumin (HSA).

Results

Conclusion