Electrospray ionization mass spectrometry of metal complexes. Gas phase formation of a binuclear copper(II)–5-Br-PADAP complex

Matsumoto, Atsushi; Fukumoto, Takao; Adachi, Hiroshi; Watarai, Hitoshi

doi:10.1016/s0003-2670(99)00222-6

Cited by 23 publications

(18 citation statements)

References 12 publications

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“…A first method (Matsumoto et al, 1999) involves the comparison of two similar metal-ligand systems: only species, which are present in both systems, are assumed not to be gas-phase products. In their work, Matsumoto et al detected a ternary copper(II)-2-(5-bromo-2-pyridilazo)-5-diethylaminophenol-acetate species, Cu 2 L 2 AcO, but they did not detect the corresponding nickel(II) species.…”

Section: Gas-phase Reactionsmentioning

confidence: 99%

Electrospray mass spectrometry (ESI‐MS) in the study of metal–ligand solution equilibria

Marco¹,

Bombi²

2005

Mass Spectrometry Reviews

326

256

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In the 20 years, since the introduction of electrospray mass spectrometry (ESI-MS), the use of this technique in various fields of inorganic, organometallic, and analytical chemistry has been steadily increasing. In this study, the application of ESI-MS to the study of metal-ligand solution equilibria is reviewed (till 2004 included). In a first section, advantages and drawbacks of ESI-MS in this type of application are described. Subsequently, a list of ca. 300 studies is reported, in which ESI-MS was used to give number and stoichiometry of the species at equilibrium, or also to estimate their stability constants. All studies are classified according to the metal ions under examination. Other related applications, such as host-guest interactions and metal ion-protein binding studies, are briefly reviewed as well.

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Section: Gas-phase Reactionsmentioning

confidence: 99%

Electrospray mass spectrometry (ESI‐MS) in the study of metal–ligand solution equilibria

Marco¹,

Bombi²

2005

Mass Spectrometry Reviews

326

256

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“…We observed the formation of dimers in the ESI-MS spectra of Pd(II)-and Cu(II)-5-Br-PADAP complexes. 3,4 It is well-known that azo dyes are ready to form dimers by an interaction between the aromatic rings of the dye molecules in crystals. 5 The bond lengths and angles in PdLCl1 and PdLCl2 were slightly different, as described in Table 3 2 + 2U12aa*bb*cos + 2U13aa*cc*cos + 2U23bb*cc*cos ).…”

mentioning

confidence: 99%

Structural Isomers in a 2-(5-Bromo-2-pyridylazo)-5-diethylaminophenolatochloropalladium(II) Crystal

2003

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2-(5-Bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP or HL) was widely used as a sensitive reagent in the determination of trace amounts of metal ions. However, there is no report on the structure of metal chelates of 5-Br-PADAP by a systematic X-ray diffraction study. Several authors reported that pyridylazo ligands having no bulky substituent gorups formed planar complexes with Pd(II) in the crystal state.1 In the case of the Pd(II)-5-Br-PADAP complex, it might have a steric hindrance in the crystal state, because of the bulky diethylamino-group in 5-Br-PADAP. Recently, we found a specific aggregation of Pd(II)-5-Br-PADAP-Cl complexes (PdLCl, Fig. 1) at the heptane/water interface. 2 The aggregate formed at the interface showed a similar electronic spectrum with that in toluene, but the structure was not determined. Therefore, it is of interest to clarify the structure of the solid state complex and to know whether the planar structure is kept in this crystal or not. In this study, we carried out an X-ray diffraction analysis of PdLCl to determine its three-dimensional structure.A purple toluene solution (about 10 ml) of 5.6 × 10 -5 M PdLCl was poured into a crystal dish and the solvent was evaporated at the room temperature. Crude crystals of PdLCl were dissolved in acetone and recrystallized at room temperature. Dark-purple and prismatic crystals were obtained. The X-ray diffraction intensities were measured at 295 K with graphite-monochromated Mo Kα radiation (λ = 0.71073 Å) on a Rigaku AFC-5R four-circle diffractometer using ω-2θ scan technique. The final lattice constants were determined by a least-squares refinement of the orientation angles of 25 centered Crystal structure of 2-(5-bromo-2-pyridylazo)-5-diethylaminophenolatochloropalladium(II) (PdLCl) has been determined by X-ray diffraction. A crystal of PdLCl was constructed by two structural isomers of PdLCl molecules, which were particularly different in the positions of the carbon atoms at the diethylamino group, having cis-like or trans-like conformation for the carbon atoms. The molecules of PdLCl in the crystal were warped by a steric hindrance of the diethylamino group.

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“…[14][15][16] Furthermore, it is often used for protic and aprotic solvents. 17 The application of ESI-MS for the analysis of transition metal complexes was reviewed in Ref.…”

Section: Introductionmentioning

confidence: 99%

Soft Ionization of Metallo-Mefenamic Using Electrospray Ionization Mass Spectrometry

Abdelhamid¹,

Wu²

2015

Mass Spectrometry Letters

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Detection of mefenamic acid (M, non-steroidal anti-inflammatory drug, NSAIDs) and its metallodrug was investigated using electrospray ionization mass spectrometry (ESI-MS) and fluorescence spectroscopy. ESI-MS data (500 µL, 1×10-3 M) revealed high detection sensitivity for the drug and metallodrug. ESI-MS spectra revealed peaks at 242, 580, and 777 Da corresponding to [M+H]+, [63Cu(M-H)2(H2O)2+H]+, and [56Fe(M-H)3+H]+, respectively. The metal:mefenamic ratios of ESI-MS spectra are in complete agreement with the fluorescence spectroscopy results (1:2 for Cu(II) and 1:3 for Fe(III)). ESI is a soft ionization technique that can be used on labile metallo-mefenamic acids and is promising for the detection of these species in environmental samples and biological fluids.

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Electrospray ionization mass spectrometry of metal complexes. Gas phase formation of a binuclear copper(II)–5-Br-PADAP complex

Cited by 23 publications

References 12 publications

Electrospray mass spectrometry (ESI‐MS) in the study of metal–ligand solution equilibria

Electrospray mass spectrometry (ESI‐MS) in the study of metal–ligand solution equilibria

Structural Isomers in a 2-(5-Bromo-2-pyridylazo)-5-diethylaminophenolatochloropalladium(II) Crystal

Soft Ionization of Metallo-Mefenamic Using Electrospray Ionization Mass Spectrometry

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