PMID- 9679296 OWN - NLM STAT- MEDLINE DCOM- 19980811 LR - 20190921 IS - 0925-2738 (Print) IS - 0925-2738 (Linking) VI - 11 IP - 2 DP - 1998 Feb TI - Accurate quantitation of water-amide proton exchange rates using the phase-modulated CLEAN chemical EXchange (CLEANEX-PM) approach with a Fast-HSQC (FHSQC) detection scheme. PG - 221-6 AB - Measurement of exchange rates between water and NH protons by magnetization transfer methods is often complicated by artifacts, such as intramolecular NOEs, and/or TOCSY transfer from C alpha protons coincident with the water frequency, or exchange-relayed NOEs from fast exchanging hydroxyl or amine protons. By applying the Phase-Modulated CLEAN chemical EXchange (CLEANEX-PM) spin-locking sequence, 135 degrees (x) 120 degrees (-x) 110 degrees (x) 110 degrees (-x) 120 degrees (x) 135 degrees (-x) during the mixing period, these artifacts can be eliminated, revealing an unambiguous water-NH exchange spectrum. In this paper, the CLEANEX-PM mixing scheme is combined with Fast-HSQC (FHSQC) detection and used to obtain accurate chemical exchange rates from the initial slope analysis for a sample of 15N labeled staphylococcal nuclease. The results are compared to rates obtained using Water EXchange filter (WEX) II-FHSQC, and spin-echo-filtered WEX II-FHSQC measurements, and clearly identify the spurious NOE contributions in the exchange system. FAU - Hwang, T L AU - Hwang TL AD - Department of Radiology School of Medicine, Johns Hopkins University, Baltimore, MD 21205-2195, USA. FAU - van Zijl, P C AU - van Zijl PC FAU - Mori, S AU - Mori S LA - eng GR - RR11115/RR/NCRR NIH HHS/United States PT - Journal Article PT - Research Support, U.S. Gov't, P.H.S. PL - Netherlands TA - J Biomol NMR JT - Journal of biomolecular NMR JID - 9110829 RN - 0 (Protons) RN - 059QF0KO0R (Water) RN - EC 3.1.31.1 (Micrococcal Nuclease) SB - IM MH - Magnetic Resonance Spectroscopy/*methods MH - Micrococcal Nuclease/*chemistry MH - Protons MH - Water/chemistry EDAT- 1998/07/29 00:00 MHDA- 1998/07/29 00:01 CRDT- 1998/07/29 00:00 PHST- 1998/07/29 00:00 [pubmed] PHST- 1998/07/29 00:01 [medline] PHST- 1998/07/29 00:00 [entrez] AID - 10.1023/a:1008276004875 [doi] PST - ppublish SO - J Biomol NMR. 1998 Feb;11(2):221-6. doi: 10.1023/a:1008276004875.