Characterization of mixtures of organic acids by ion-exclusion partition chromatography-mass spectrometry

Pacholec, F.; Eaton, D. R.; Rossi, David T.

doi:10.1021/ac00125a051

Cited by 26 publications

(9 citation statements)

References 8 publications

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“…This study explores the use of LC/MS for the routine analysis of low molecular weight carboxylic acids. MS detection of carboxylic acids after their separation by liquid chromatography was reported by Pacholec 8. Detection limits of 10 ppm were obtained for glycolic, acetic, propionic and butyric acids.…”

mentioning

confidence: 98%

Improved liquid chromatography/mass spectrometric analysis of low molecular weight carboxylic acids by ion exclusion separation with electrospray ionization

Gamoh¹,

Saitoh²,

Wada³

2003

Rapid Comm Mass Spectrometry

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An improved, simple and sensitive analytical method for low molecular weight organic acids has been developed. A mixture of acetic, propionic, butyric, glycolic, lactic, 2-hydroxybutyric, malonic, succinic, glutaric, tartaric and citric acids was separated on a semi-rigid styrene-divinylbenzene copolymer-based H-type cation-exchange resin (ULTRON PS-80H) based on an ion exclusion chromatographic (IEC) mechanism, with detection using electrospray ionization mass spectrometry (ESI-MS). Formic or acetic acid was used as a mobile phase to separate the carboxylic acids within 15 min. For liquid chromatography/mass spectrometry (LC/MS), the ESI interface was used in both positive and negative ionization mode. ESI produced reasonable signals from positive ions, [M+NH(4)](+), of acetic, propionic and butyric acids and from negative ions, [M-H](-), of glycolic, lactic, 2-hydroxybutyric, malonic, succinic, glutaric, tartaric and citric acids. The effects of ionization parameters, source temperature, capillary voltage and cone voltage, on sensitivity and linearity were examined. Linear plots of peak area versus concentration were obtained over the range 0.1-20 ppm for MS detection. The detection limits of the target carboxylic acids calculated at signal-to-noise (S/N) ratio of 3 ranged from 9 to 59 ppb. The reproducibility of retention times and peak areas were 0.55-1.25 and 0.85-2.45%, respectively.

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mentioning

confidence: 98%

Improved liquid chromatography/mass spectrometric analysis of low molecular weight carboxylic acids by ion exclusion separation with electrospray ionization

Gamoh¹,

Saitoh²,

Wada³

2003

Rapid Comm Mass Spectrometry

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“…The successful analysis of acidic pharmaceuticals in biological fluids using IC with sensitive fluorescence detection after labeling was reported by Muhammad et al [100]. A further increase in sensitivity is obtained when coupling IC with MS [109] upon further improvements of the interfaces. Recently, Stoll [110] summarized the state of the art of IC-MS.…”

Section: Ion Chromatographymentioning

confidence: 86%

Trends in sample preparation and separation methods for the analysis of very polar and ionic compounds in environmental water and biota samples

2020

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Recent years showed a boost in knowledge about the presence and fate of micropollutants in the environment. Instrumental and methodological developments mainly in liquid chromatography coupled to mass spectrometry hold a large share in this success story. These techniques soon complemented gas chromatography and enabled the analysis of more polar compounds including pesticides but also household chemicals, food additives, and pharmaceuticals often present as traces in surface waters. In parallel, sample preparation techniques evolved to extract and enrich these compounds from biota and water samples. This review article looks at very polar and ionic compounds using the criterion log P ≤ 1. Considering about 240 compounds, we show that (simulated) log D values are often even lower than the corresponding log P values due to ionization of the compounds at our reference pH of 7.4. High polarity and charge are still challenging characteristics in the analysis of micropollutants and these compounds are hardly covered in current monitoring strategies of water samples. The situation is even more challenging in biota analysis given the large number of matrix constituents with similar properties. Currently, a large number of sample preparation and separation approaches are developed to meet the challenges of the analysis of very polar and ionic compounds. In addition to reviewing them, we discuss some trends: for sample preparation, preconcentration and purification efforts by SPE will continue, possibly using upcoming mixed-mode stationary phases and mixed beds in order to increase comprehensiveness in monitoring applications. For biota analysis, miniaturization and parallelization are aspects of future research. For ionic or ionizable compounds, we see electromembrane extraction as a method of choice with a high potential to increase throughput by automation. For separation, predominantly coupled to mass spectrometry, hydrophilic interaction liquid chromatography applications will increase as the polarity range ideally complements reversed phase liquid chromatography, and instrumentation and expertise are available in most laboratories. Two-dimensional applications have not yet reached maturity in liquid-phase separations to be applied in higher throughput. Possibly, the development and commercial availability of mixed-mode stationary phases make 2D applications obsolete in semi-targeted applications. An interesting alternative will enter routine analysis soon: supercritical fluid chromatography demonstrated an impressive analyte coverage but also the possibility to tailor selectivity for targeted approaches. For ionic and ionizable micropollutants, ion chromatography and capillary electrophoresis are amenable but may be used only for specialized applications such as the analysis of halogenated acids when aspects like desalting and preconcentration are solved and the key advantages are fully elaborated by further research.

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“…The mobile phase selected for thermospray LC/MS was 0.001N HCI because it is considerably more volatile than 0.01 H2SO,. A mobile phase of 0.001N HCI has been used with some success by Pacholec (Pacholec et al 1986) in characterizing mixtures of organic acids by ion-exclusion partition • chromatography-mass spectrometry. Water is flushed through the entire system at the end of each day to prevent damage to instrument components from the HCI.…”

Section: Analysis Of Waste Sample Using Thermospray Lc/msmentioning

confidence: 99%

Flammable gas safety program. Analytical methods development: FY 1993 progress report

Campbell¹,

Clauss²,

Grant³

et al. 1994

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• Six samples of core segments from Tank 101-SY, obtained during the window E core sampling, have been analyzed for organic constituents. Four of the samples were from the upper region, or convective layer, of the tank and two were from the lower, nonconvective layer. The samples were analyzed for chelators, chelator fragments, and several carboxylic acids by derivatization gas chromatography/mass spectrometry (GC/MS). The major components detected were ethylenediaminetetraacetie acid (EDTA), nitroso-iminodiacetic acid (NIDA), nitrilotriacetic acid (NTA), citric acid (CA), succinic acid (SA), and ethylenediaminetriacetic acid ('ED3A). The chelator of highest concentration was EDTA in all six samples analyzed. Liquid chromatography (LC) was used to quantitate low molecular weight acids (LMWA) including oxalic, formic, glyeolic, and acetic acids, which are present in the waste as acid salts. From 23 to 61% of the total organic carbon (TOC) in the samples analyzed was accounted for by these acids. Oxalate constituted approximately 40% of the TOC in the nonconvective layer samples. Oxalate was found to be approximately 3 to 4 times higher in concentration in the nonconvective layer than in the convective layer. During FY 1993, LC methods for analyzing LWMA, and two chelators N-(2-hydroxyethyl) ethylenediaminetriacetic acid and EDTA, were transferred to personnel in the Analytical Chemistry Laboratory and the 222-S laboratory.

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Characterization of mixtures of organic acids by ion-exclusion partition chromatography-mass spectrometry

Cited by 26 publications

References 8 publications

Improved liquid chromatography/mass spectrometric analysis of low molecular weight carboxylic acids by ion exclusion separation with electrospray ionization

Improved liquid chromatography/mass spectrometric analysis of low molecular weight carboxylic acids by ion exclusion separation with electrospray ionization

Trends in sample preparation and separation methods for the analysis of very polar and ionic compounds in environmental water and biota samples

Flammable gas safety program. Analytical methods development: FY 1993 progress report

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