核磁中内标选择.pdf

Journal of Pharmaceutical and Biomedical Analysis 52 (2010) 645–651 Contents lists available at ScienceDirect Journal of Pharmaceutical and Biomedical Analysis j o u rn al h omepage: w w w. elsev /locate/jpba Survey and qualification of internal standards for quantification by 1H NMR spectroscopy Torgny Rundlöf a,∗ , Marie Mathiasson a , Somer Bekiroglu b,1, Birgit Hakkarainen a,b , Tim Bowden c , Torbjörn Arvidsson a,b a Medical Products Agency, P.O. Box 26, SE-75103 Uppsala, Sweden b Division of Analytical Pharmaceutical Chemistry, Department of Medicinal Chemistry, Uppsala University, Biomedical Centre, Box 574, SE-751 23, Uppsala, Sweden c Division of Polymer Chemistry, Department of Materials Chemistry, Uppsala University, Ångström Laboratory, Box 538, SE-751 21 Uppsala, Sweden a r t i c l e i n f o a b s t r a c t Article history: In quantitative NMR (qNMR) selection of an appropriate internal standard proves to be crucial. In this Received 23 November 2009 study, 25 candidate compounds considered to be potent internal standards were investigated with Received in revised form 29 January 2010 respect to the ability of providing unique signal chemical shifts, purity, solubility, and ease of use. The 1H Accepted 4 February 2010 chemical shift (ı) values, assignments, multiplicities and number of protons (for each signal), appropri- Available online 11 February 2010 ateness (as to be used as internal standards) in four different deuterated solvents (D O, DMSO-d , CD OD,