Anal. Chem. （离子交换色谱-质谱-ICP原子发射光谱-核磁共振联用）.pdf

Article pubs.acs.org/ac Speciation of Inositol Phosphates in Lake Sediments by Ion- Exchange Chromatography Coupled with Mass Spectrometry, Inductively Coupled Plasma Atomic Emission Spectroscopy, and 31P NMR Spectroscopy Julia V. Paraskova, † Charlotte Jørgensen,‡ Kasper Reitzel,‡ Jean Pettersson, † Emil Rydin,† and Per J. R. Sjoberg*̈ ,† †Department of Chemistry−Biomedical Centre, Uppsala University, P.O. Box 599, S-751 24 Uppsala, Sweden ‡Department of Biology, University of Southern Denmark, Campusvej 55, 5230 Odense, Denmark ABSTRACT: A method for the detection and speciation of inositol phosphates (InsPn) in sediment samples was tested, utilizing oxalate−oxalic acid extraction followed by determi- nation by high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC−MS/MS) using electrospray ionization (ESI) in negative mode. The chromato- graphic separation was carried out using water and ammonium bicarbonate as mobile phase in gradient mode. Data acquisition under MS/MS was attained by multiple reaction monitoring. The technique provided a sensitive and selective detection of InsPn in sediment samples. Several forms of InsPn in the oxalate−oxalic acid extracted sediment were identified. InsP6 was the dominating form constituting 0.250 mg P/g DW (dry weight); InsP5 and InsP4 constituted 0.045 and 0.014 mg P/g DW, respectively. The detection limit of the LC−ESI-MS/MS method was 0.03 μM InsP , which is superior to the currently used method for the identification of InsP , 31P nuclear magnetic