A rapid HPLC method for the determination of carboxylic acids in human urine using a monolithic column

Šperlingová, Ilona; Dabrowská, Ludmila; Stránský, Vladimír; Tichý, M

doi:10.1007/s00216-003-2289-z

Cited by 24 publications

(15 citation statements)

References 9 publications

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“…Briefly, 2 mL of water containing each of the seven substances were treated as indicated above, extracted with 0.5 mL of chloroform and analyzed using a GC-MS detector. Moreover, 20 μL of the derivatized water, before the extraction in chloroform, was injected into a highperformance liquid chromatograph (HPLC) with an ultraviolet detector, under the conditions indicated in the literature (Sperlingova et al, 2004), to determine the amount of carboxylic acid not converted to corresponding methylester. The comparison between the quantitative GC-MS and HPLC data gave an indication of the yield of the methylation reaction (>95% for all compounds).…”

Section: Resultsmentioning

confidence: 99%

Determination of organic acids in urine by solid‐phase microextraction and gas chromatography–ion trap tandem mass spectrometry previous ‘in sample’ derivatization with trimethyloxonium tetrafluoroborate

Pacenti

Dugheri

Villanelli

et al. 2008

Biomedical Chromatography

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A method for the determination of the organic acids directly in the urine employing derivatization with trimethyloxonium tetrafluoroborate as a methylating agent and sequential extraction by head space and direct immersion/solid phase microextraction is reported. Furoic acid, hippuric acid, methylhippuric acid, mandelic acid, phenylglyoxylic acid and trans, trans muconic acid contained in urine and proposed by the American Conference of Governmental Industrial Hygienists as biological exposure indices were determined after a fast and economically convenient preparation step and sensitive gas chromatography-ion trap-mass spectrometry/tandem mass spectrometry analysis. Urine is rather a complex sample and hence the acquisition method required specific GC-MS instrumentation capable of supporting the changeover, fully automated during a single chromatographic separation, from mass to tandem mass spectrometry and both chemical and electron ionization modes. The automation of the analytical method provides a number of advantages, including reduced analysis time for both routine analysis and method development, and greater reproducibility. The equilibrium and kinetics of this substances vs head space/direct immersion-solid phase microextraction were investigated and evaluated theoretically.

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Section: Resultsmentioning

confidence: 99%

Determination of organic acids in urine by solid‐phase microextraction and gas chromatography–ion trap tandem mass spectrometry previous ‘in sample’ derivatization with trimethyloxonium tetrafluoroborate

Pacenti

Dugheri

Villanelli

et al. 2008

Biomedical Chromatography

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show abstract

“…Both methods have a chromatographic time of r2.0 min [9,10] while methods using conventional particulate columns have a run time ranging from 7.0 to 20.0 min [9]. A direct comparison between HPLC methods using LiChrosorb RP-18 and Chromolith RP-18 columns for carboxylic acid shows a 17 min reduction (28 min versus 11 min) in chromatography time [43]. An HPLC method using Chromolith Performance RP-18e column has a similar sensitivity for retinol and a-tocopherol (0.07 and 0.3 mmol/L, respectively) compared to an HPLC method using Pecosphere C-18 particulate column [50].…”

Section: Chromatography Time and Mobile Phase Consumptionmentioning

confidence: 98%

“…The original method had a run time of 11 min. The chromatographic time was shortened to 5 min for measuring five carboxylic acids because methylhippuric acid was not present in human urine [43]. The UV detector is set at 220, 225, and 254 nm in order to have the best signal for all compounds.…”

Section: Trace Compound Analysismentioning

confidence: 99%

Applications of monolithic columns in liquid chromatography‐based clinical chemistry assays

Bunch

Wang

2011

J of Separation Science

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Monolithic columns have slowly been applied to HPLC methods for clinical chemistry testing in the last 10 years. The application areas include therapeutic drug monitoring, drugs of abuse, vitamins, porphyrins, and steroids. In comparison with conventional particulate columns, the monolithic columns may offer shorter chromatography time, more robustness, and better resolution for certain analytes. The potential drawback of large mobile phase consumption may be improved with smaller id columns, which are currently on the market. Methods covered in this review are those searchable in PubMed up to December 2010. This review highlights the emergence of monolithic column technology in HPLC methods used for clinical chemistry testing. The goals of this review are threefold: (i) To identify the areas of clinical chemistry that analytical monolithic columns have been used in HPLC methods. (ii) To demonstrate the application of analytical monolithic columns in HPLC methods using different detection systems. (iii) To discuss the advantages and limitations of the monolithic columns compared with particulate columns in the clinical chemistry applications.

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“…For accurate and comprehensive evaluation of combined exposure, simultaneous determination of these urinary metabolites is desired for routine biological monitoring. Several simultaneous determination methods for these urinary metabolites have been reported, including gas chromatography‐mass spectrometry (GC‐MS), high‐performance capillary electrophoresis (HPCE), high‐performance liquid chromatography‐ultraviolet (HPLC‐UV) detection, high‐performance liquid chromatography‐hybrid quadrupole time‐of‐flight mass spectrometry (HPLC‐QqTOF‐MS), and ultra‐high‐performance liquid chromatography‐electrospray ionization tandem mass spectrometry (UPLC‐ESI‐MS/MS) . However, each of these methods has disadvantages.…”

Section: Introductionmentioning

confidence: 99%

Direct methyl esterification with 2,2‐dimethoxypropane for the simultaneous determination of urinary metabolites of toluene, xylene, styrene, and ethylbenzene by gas chromatography‐mass spectrometry

Takeuchi

Namera

Sakui

et al. 2019

Journal of Occupational Health

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Objectives The purpose of this study was to develop a simple and accurate gas chromatography‐mass spectrometry (GC‐MS) method for simultaneous determination of four urinary metabolites from four organic solvents, that is, hippuric acid (HA) from toluene, methylhippuric acid (MHA) from xylene, and mandelic acid (MA) and phenylglyoxylic acid (PGA) from styrene or ethylbenzene for biological monitoring. Methods The four metabolites were directly methyl‐esterified with 2,2‐dimethoxypropane and analyzed using GC‐MS. The proposed method was validated according to the US Food and Drug Administration guidance. The accuracy of the proposed method was confirmed by analyzing a ClinChek ® —Control for occupational medicine (RECIPE Chemicals +Instruments GmbH). Results Calibration curves showed linearity in the concentration range of 10‐1000 mg/L for each metabolite, with correlation coefficients >0.999. For each metabolite, the limits of detection and quantification were 3 mg/L and 10 mg/L, respectively. The recovery was 93%‐117%, intraday accuracy, expressed as the deviation from the nominal value, was 92.7%‐103.0%, and intraday precision, expressed as the relative standard deviation (RSD), was 1.3%‐4.7%. Interday accuracy and precision were 93.4%‐104.0% and 1.2%‐9.5%, respectively. The analytical values of ClinChek obtained using the proposed method were sufficiently accurate. Conclusions The proposed method is a simple and accurate which is suitable for routine analyses that could be used for biological monitoring of occupational exposure to four organic solvents.

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A rapid HPLC method for the determination of carboxylic acids in human urine using a monolithic column

Cited by 24 publications

References 9 publications

Determination of organic acids in urine by solid‐phase microextraction and gas chromatography–ion trap tandem mass spectrometry previous ‘in sample’ derivatization with trimethyloxonium tetrafluoroborate

Determination of organic acids in urine by solid‐phase microextraction and gas chromatography–ion trap tandem mass spectrometry previous ‘in sample’ derivatization with trimethyloxonium tetrafluoroborate

Applications of monolithic columns in liquid chromatography‐based clinical chemistry assays

Direct methyl esterification with 2,2‐dimethoxypropane for the simultaneous determination of urinary metabolites of toluene, xylene, styrene, and ethylbenzene by gas chromatography‐mass spectrometry

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