Gradient ion-pair chromatographic method for the determination of iron N,N′-ethylenediamine-di-(2-hydroxy-5-sulfophenylacetate) by high performance liquid chromatography–atmospheric pressure ionization electrospray mass spectrometry

García‐Marco, Sonia; Cremonini, Mauro Andrea; Esteban, Pedro; Yunta, Felipe; Hernández‐Apaolaza, Lourdes; Placucci, Giuseppe; Lucena, Juan J.

doi:10.1016/j.chroma.2004.12.028

Cited by 17 publications

(15 citation statements)

References 18 publications

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“…The chemical characterization of fertilizers containing synthetic Fe(III)-chelates of EDTA, DTPA, EDDHA, EDDHMA, EDDHSA, and EDDCHA has been dealt with using HPLC-ESI/MS [21], although this study provided very limited analytical information, reporting only chromatographic retention times and m/z values for the [M Ϫ H] Ϫ1 ions of each chelate. Also, HPLC-ESI/MS was used to characterize Fe(III)-EDDHSA commercial fertilizers, finding a peak with m/z attributable to an Fe(III)-EDDHSA condensation product along with the peak of the active ingredient (Fe(III)-EDDHSA) [22].…”

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Determination of synthetic ferric chelates used as fertilizers by liquid chromatography-electrospray/mass spectrometry in agricultural matrices

Álvarez‐Fernández

Orera

Abadı́a

et al. 2007

J. Am. Soc. Mass Spectrom.

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A high-performance liquid chromatography-electrospray ionization/mass spectrometry (time of flight) method has been developed for the simultaneous determination of synthetic . The average intraday repeatability values were ϳ0.5 and 5% for retention time and peak area, respectively, whereas the interday repeatability values were ϳ0.7 and 8% for retention time and peak area, respectively. The method was validated using four different agricultural matrices, including nutrient solution, irrigation water, soil solution, and plant xylem exudates, spiked with Fe(III)-chelate standards and their stable isotope-labeled corresponding chelates. Analyte recoveries found were in the ranges 92-101% (nutrient solution), 89 -102% (irrigation water), 82-100% (soil solution), and 70 -111% (plant xylem exudates). Recoveries depended on the analyte, with Fe(III)-EDTA and Fe(III)-DTPA showing the lowest recoveries (average values of 87 and 88%, respectively, for all agricultural matrices used), whereas for other analytes recoveries were between 91 and 101%. The method was also used to determine the real concentrations of Fe(III)-chelates in commercial fertilizers. Furthermore, the method is also capable of resolving two more synthetic Fe(III)-chelates, Fe(III)-EDDHSA and Fe(III)-ED-DCHA, whose exact quantification is not currently possible because of lack of commercial standards. (J Am Soc Mass Spectrom 2007, 18, 37-47)

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Determination of synthetic ferric chelates used as fertilizers by liquid chromatography-electrospray/mass spectrometry in agricultural matrices

Álvarez‐Fernández

Orera

Abadı́a

et al. 2007

J. Am. Soc. Mass Spectrom.

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“…This study opens the possibility of applying HPLC/ESI‐CID‐MS 2 (QTOF) analyses to identify Fe‐containing byproducts in commercial synthetic Fe(III)‐chelate fertilizers. The most common approaches to identify impurities in fertilizers have been HPLC/UV‐Vis15, 19 or HPLC/ESI‐MS26 direct analyses and NMR analyses of deferrated fertilizers 23, 24. Since the HPLC/UV‐Vis and HPLC/ESI‐MS direct analyses provide limited structural information compared with NMR, the identity of the impurities has been putatively assigned in most cases, with only a few confirmations through the synthesis of standards (e.g.…”

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confidence: 99%

“…A novel method using cyanide transfer agents instead of HCN has been developed, although it has not yet been scaled up for industrial applications 16. Current industrial synthesis processes17, 18 lead to products which often contain starting chemicals as well as reaction byproducts 15, 19–26. For this reason, a common characteristic of these fertilizers is the occurrence of a significant water‐soluble Fe fraction not bound to the authorized chelating agents 20–22.…”

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“…This is especially relevant in fertilizers containing phenolic groups in the chelating agent structure, where 40–50% of the total Fe can be bound to unknown products 22. The occurrence of positional isomers and poly‐condensate products in Fe(III)‐ o,o EDDHA, Fe(III)‐EDDHMA and Fe(III)‐EDDHSA fertilizers was suggested first by HPLC/UV‐Vis, and later confirmed by one‐ and two‐dimensional nuclear magnetic resonance (NMR) and electrospray ionization (ESI) mass spectrometry (MS) 15, 19, 23, 24, 26. For instance, 14–30% of the water‐soluble Fe content found in Fe(III)‐ o,o EDDHA fertilizers actually corresponds to Fe(III)‐ o,p EDDHA.…”

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confidence: 99%

“…Until now, MS studies have focused mainly on the quantification of the active ingredients of Fe(III)‐chelate fertilizers using exact molecular masses26–29 and isotopic signatures 30. However, significant structural information can be obtained from collision‐induced dissociation (CID) MS/MS, that provides molecular fragmentation patterns.…”

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Electrospray ionization collision‐induced dissociation mass spectrometry: a tool to characterize synthetic polyaminocarboxylate ferric chelates used as fertilizers

Orera¹,

Orduna²,

Abadı́a³

et al. 2009

Rapid Comm Mass Spectrometry

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Fertilizers based on synthetic polyaminocarboxylate ferric chelates have been known since the 1950s to be successful in supplying Fe to plants. In commercial Fe(III)‐chelate fertilizers, a significant part of the water‐soluble Fe‐fraction consists of still uncharacterized Fe byproducts, whose agronomical value is unknown. Although collision‐induced dissociation (CID) tandem mass spectrometry (MS/MS) is a valuable tool for the identification of such compounds, no fragmentation data have been reported for most Fe(III)‐chelate fertilizers. The aim of this study was to characterize the CID‐MS2 fragmentation patterns of the major synthetic Fe(III)‐chelates used as Fe‐fertilizers, and subsequently use this technique for the characterization of commercial fertilizers. Quadrupole‐time‐of‐flight (QTOF) and spherical ion trap mass analyzers equipped with an electrospray ionization (ESI) source were used. ESI‐CID‐MS2 spectra obtained were richer when using the QTOF device. Specific differences were found among Fe(III)‐chelate fragmentation patterns, even in the case of positional isomers. The analysis of a commercial Fe(III)‐chelate fertilizer by high‐performance liquid chromatography (HPLC) coupled to ESI‐MS(QTOF) revealed two previously unknown, Fe‐containing compounds, that were successfully identified by a comprehensive comparison of the ESI‐CID‐MS2(QTOF) spectra with those of pure chelates. This shows that HPLC/ESI‐CID‐MS2(QTOF), along with the Fe(III)‐chelate fragmentation patterns, could be a highly valuable tool to directly characterize the water‐soluble Fe fraction in Fe(III)‐chelate fertilizers. This could be of great importance in issues related to crop Fe‐fertilization, both from an agricultural and an environmental point of view. Copyright © 2009 John Wiley & Sons, Ltd.

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Current literature in mass spectrometry

2005

J. Mass Spectrom.

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In order to keep subscribers up‐to‐date with the latest developments in their field, John Wiley & Sons are providing a current awareness service in each issue of the journal. The bibliography contains newly published material in the field of mass spectrometry. Each bibliography is divided into 11 sections: 1 Books, Reviews & Symposia; 2 Instrumental Techniques & Methods; 3 Gas Phase Ion Chemistry; 4 Biology/Biochemistry: Amino Acids, Peptides & Proteins; Carbohydrates; Lipids; Nucleic Acids; 5 Pharmacology/Toxicology; 6 Natural Products; 7 Analysis of Organic Compounds; 8 Analysis of Inorganics/Organometallics; 9 Surface Analysis; 10 Environmental Analysis; 11 Elemental Analysis. Within each section, articles are listed in alphabetical order with respect to author (4 Weeks journals ‐ Search completed at 6th. July 2005)

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Gradient ion-pair chromatographic method for the determination of iron N,N′-ethylenediamine-di-(2-hydroxy-5-sulfophenylacetate) by high performance liquid chromatography–atmospheric pressure ionization electrospray mass spectrometry

Cited by 17 publications

References 18 publications

Determination of synthetic ferric chelates used as fertilizers by liquid chromatography-electrospray/mass spectrometry in agricultural matrices

Determination of synthetic ferric chelates used as fertilizers by liquid chromatography-electrospray/mass spectrometry in agricultural matrices

Electrospray ionization collision‐induced dissociation mass spectrometry: a tool to characterize synthetic polyaminocarboxylate ferric chelates used as fertilizers

Current literature in mass spectrometry

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