Redox speciation of iron, manganese, and copper in cerebrospinal fluid by strong cation exchange chromatography - sector field inductively coupled plasma mass spectrometry.

Title Redox speciation of iron, manganese, and copper in cerebrospinal fluid by strong cation exchange chromatography - sector field inductively coupled plasma mass spectrometry.
Authors N. Solovyev; M. Vinceti; P. Grill; J. Mandrioli; B. Michalke
Journal Anal Chim Acta
DOI 10.1016/j.aca.2017.03.040
Abstract

A new method of simultaneous redox speciation of iron (II/III), manganese (II/III), and copper (I/II) in cerebrospinal fluid (CSF) has been designed. For the separation of redox species strong cation exchange chromatography (SCX) with isocratic elution was employed. Species were detected using inductively coupled plasma sector field mass spectrometry (ICP-sf-MS), operating at medium resolution. The following parameters were optimized: analytical column, eluent composition and pH, CSF injection volume and dilution factor. Analytical column Dionex IonPac CS5A RFIC 4*250 mm was found to retain and separate species of interest the most effectively under the isocratic elution with a buffer, containing 50 mM ammonium citrate, 7.0 mM pyridine-2,6-dicarboxylic acid at pH = 4.2 and flow rate of 0.8 L min(-1). Injection volume of 50 ?L with CSF sample dilution of 1/3 (v/v) with the eluent was shown to result in minimal matrix suppression. For species identification, retention time matching with standards was used. The stability of metalloproteins (ferritin, transferrin, and ceruloplasmin) under elution conditions was evaluated. For the quantification of redox species, external calibration was employed. To avoid column contamination, a blank was run after measurement and all quantification values were blank subtracted. For recovery checks, species quantification data was verified against total content of an element, measured by dynamic reaction cell ICP-MS. Recoveries (sum of quantified species vs. total element determinations) were 82.5 ± 22% (Mn), 92 ± 11% (Fe), and 88.7 ± 12% (Cu). The method was tested using 38 real CSF samples. Limits of detection (3?) for the CSF samples were 0.5 ?g L(-1), 0.6 ?g L(-1), and 0.8 ?g L(-1) for Fe, Mn, and Cu species, respectively. Retention time precision was 1-7.5% (as RSD), whereas peak area RSDs were in the range 5-11%, both depending on the species.

Citation N. Solovyev; M. Vinceti; P. Grill; J. Mandrioli; B. Michalke.Redox speciation of iron, manganese, and copper in cerebrospinal fluid by strong cation exchange chromatography - sector field inductively coupled plasma mass spectrometry.. Anal Chim Acta. 2017;973:2533. doi:10.1016/j.aca.2017.03.040

Related Elements

Copper

See more Copper products. Copper Bohr Model Copper (atomic symbol: Cu, atomic number: 29) is a Block D, Group 11, Period 4 element with an atomic weight of 63.546. The number of electrons in each of copper's shells is 2, 8, 18, 1 and its electron configuration is [Ar]3d10 4s1. The copper atom has a radius of 128 pm and a Van der Waals radius of 186 pm. Copper was first discovered by Early Man prior to 9000 BC. In its elemental form, copper has a reddish-orange metallic and lustrous appearance. Of all pure metals, only silver Elemental Copperhas a higher electrical conductivity. The origin of the word copper comes from the Latin word 'cuprium' which translates as "metal of Cyprus," as the Mediterranean island of Cyprus was known as an ancient source of mined copper..

Iron

See more Iron products. Iron (atomic symbol: Fe, atomic number: 26) is a Block D, Group 8, Period 4 element with an atomic weight of 55.845. The number of electrons in each of Iron's shells is 2, 8, 14, 2 and its electron configuration is [Ar] 3d6 4s2. Iron Bohr ModelThe iron atom has a radius of 126 pm and a Van der Waals radius of 194 pm. Iron was discovered by humans before 5000 BC. In its elemental form, iron has a lustrous grayish metallic appearance. Iron is the fourth most common element in the Earth's crust and the most common element by mass forming the earth as a whole. Iron is rarely found as a free element, since it tends to oxidize easily; it is usually found in minerals such as magnetite, hematite, goethite, limonite, or siderite.Elemental Iron Though pure iron is typically soft, the addition of carbon creates the alloy known as steel, which is significantly stronger.

Manganese

See more Manganese products. Manganese (atomic symbol: Mn, atomic number: 25) is a Block D, Group 7, Period 4 element with an atomic weight of 54.938045. Manganese Bohr ModelThe number of electrons in each of Manganese's shells is [2, 8, 13, 2] and its electron configuration is [Ar] 3d5 4s2. The manganese atom has a radius of 127 pm and a Van der Waals radius of 197 pm. Manganese was first discovered by Torbern Olof Bergman in 1770 and first isolated by Johann Gottlieb Gahn in 1774. In its elemental form, manganese has a silvery metallic appearance. Elemental ManganeseIt is a paramagnetic metal that oxidizes easily in addition to being very hard and brittle. Manganese is found as a free element in nature and also in the minerals pyrolusite, braunite, psilomelane, and rhodochrosite. The name Manganese originates from the Latin word mangnes, meaning "magnet."