Simultaneous determination of some phthalate metabolites, parabens and benzophenone-3 in urine by ultra high pressure liquid chromatography tandem mass spectrometry

Dewalque, Lucas; Pirard, Catherine; Dubois, Nathalie; Charlier, Corinne

doi:10.1016/j.jchromb.2014.01.002

Cited by 85 publications

(71 citation statements)

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“…The modified gradient (of a previously reported method [32]; see BHPLC conditions^under BMaterials and methods^) we used completed the separation of paraben stuctural isomers. The addition of 0.1 % acetic acid to the mobile phase was essential for the retention of phthalate metabolites and their proper separation [34,37,38]. Besides, the acidic mobile phase suppresses the analyte signal, in the negative ESI mode, and increases the iLOD for all studied analytes (Table 2) and particularly for BPA [34,37,38].…”

Section: Resultsmentioning

confidence: 99%

“…Optimisation of mass spectrometry ESI is the widely used ionisation technique due to its enhanced sensitivity, the low flow rates it requires and its capability to ionise a wide range of analytes [31,34,37,38]. Although sensitivity was at same levels with APCI, the need for frequent maintenance of this ionisation source (cleaning/replacing corona needles, replacing sample tube) and the significantly larger solvent consumption led us to use ESI.…”

Section: Resultsmentioning

confidence: 99%

“…The addition of 0.1 % acetic acid to the mobile phase was essential for the retention of phthalate metabolites and their proper separation [34,37,38]. Besides, the acidic mobile phase suppresses the analyte signal, in the negative ESI mode, and increases the iLOD for all studied analytes (Table 2) and particularly for BPA [34,37,38]. A chromatogram of a pooled urine sample, spiked with 100 ng of all analytes, is shown in Fig.…”

Section: Resultsmentioning

confidence: 99%

“…Treatment and clean-up of the samples was based on previous work [33] but modified as follows: Urine samples (1 mL) were transferred to a Falcon tube (polypropylene, 15 mL) and spiked with 100 ng 13 C 4 -labelled phthalate metabolites and 13 C 4 -labelled 4-methylumbelliferrone, 20 ng 13 C 6 -labelled PBs and 200 ng 4-methylumbelliferryl glucuronide. The hydrolysis step, with use of E. coli or Helix pomatia β-glucuronidase, has been reported and evaluated in numerous publications [34,36,37]. We have used the E. coli β-glucuronidase hydrolysis as follows: E. coli β-glucuronidase buffer (prepared daily, per sample: 10 μL E. coli β-glucuronidase and 250 μL ammonium acetate buffer, 1 M in aqueous solution, pH 6.5) was added to the urine samples, and hydrolysis was completed at 37°C for 90 min.…”

Section: Sample Preparationmentioning

confidence: 99%

“…Several methods suitable for measuring phthalate metabolites, BPA, or PBs have been published, but none of them measure all three compound classes [30][31][32][33][34][35]. Furthermore, only ultra performance liquid chromatography (UPLC) has been reported to sufficiently separate the structural isomers of propyl and butyl paraben [30].…”

Section: Introductionmentioning

confidence: 99%

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Determination and separation of bisphenol A, phthalate metabolites and structural isomers of parabens in human urine with conventional high-pressure liquid chromatography combined with electrospray ionisation tandem mass spectrometry

et al. 2015

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Phthalates, bisphenol A (BPA) and parabens (PBs), organic chemicals widely used in everyday products, are considered to be endocrine disruptors. We propose a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of seven phthalate metabolites, six PBs and BPA in human urine. All three categories of the above endocrine disruptors were simultaneously extracted from 1 mL of human urine using solid phase extraction. In addition, with a conventional reversed phase LC column, we achieved for the first time the separation of three pairs of structural isomers, namely iso-/n-butyl paraben, propyl paraben and monobutyl phthalate. LC-MS/MS was operated and tested in both electrospray ionisation (ESI) and atmospheric pressure chemical ionisation (APCI). ESI was selected for the analysis due to its superior stability and repeatability. The method limit of detection (mLOD), achieved for a single set of high-performance LC conditions, ranged from 0.01 to 0.84 ng/mL for phthalate metabolites, from 0.06 to 0.24 ng/mL for PBs and was 2.01 ng/mL for BPA. Derivatisation of BPA with dansyl chloride lowered its mLOD to 0.007 ng/mL. Blank contamination was non-detectable. The present method was successfully applied for the analysis of the above-mentioned compounds in 80 male human urine samples.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Sample Preparationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Determination and separation of bisphenol A, phthalate metabolites and structural isomers of parabens in human urine with conventional high-pressure liquid chromatography combined with electrospray ionisation tandem mass spectrometry

et al. 2015

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A novel UPLC‐MS/MS method for sensitive quantitation of boldine in plasma, a potential anti‐inflammatory agent: application to a pharmacokinetic study in rats

Zeng

Liu

Chen

et al. 2014

Biomedical Chromatography

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Boldine is a potential anti-inflammatory agent found in several different plants. Published bioanalytical methods using HPLC with ultraviolet and fluorescent detection lacked enough sensitivity and required tedious sample preparation procedures. Herein, we describe the development of a novel ultra-high performance LC with MS/MS for determination of boldine in plasma. Boldine in plasma was recovered by liquid-liquid extraction using 1 mL of methyl tert-butyl ether. Chromatographic separation was performed on a C18 column at 45°C, with a gradient elution consisting of acetonitrile and water containing 0.1% (v/v) formic acid at a flow rate of 0.3 mL/min. The detection was performed on an electrospray triple-quadrupole MS/MS by positive ion multiple reaction monitoring mode. Good linearity (r(2) > 0.9926) was achieved in a concentration range of 2.555-2555 ng/mL with a lower limit of quantification of 2.555 ng/mL for boldine. The intra- and inter-day precisions of the assay were 1.2-6.0 and 1.8-7.4% relative standard deviation with an accuracy of -6.0-8.0% relative error. This newly developed method was successfully applied to a single low-dose pharmacokinetic study in rats and was demonstrated to be simpler and more sensitive than the published methods, allowing boldine quantification in reduced plasma volume.

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Analytical method for urinary metabolites as biomarkers for monitoring exposure to phthalates by gas chromatography/mass spectrometry

Yoshida

2017

Biomedical Chromatography

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Phthalates, widely used as plasticizers, have been detected in indoor air, but there have been few reports on methods of analyzing urinary metabolites as biomarkers to monitor exposure to di-n-pentyl phthalate or di-n-hexyl phthalate. Presented here is a cost-effective and sensitive analytical method for the determination of urinary metabolites of phthalates containing these two compounds. Nine urinary phthalate metabolites were enzymatically hydrolyzed and extracted with toluene: monomethyl phthalate, monoethyl phthalate, monoisobutyl phthalate, mono-n-butyl phthalate, mono-n-pentyl phthalate, mono-n-hexyl phthalate, monocyclohexyl phthalate, monobenzyl phthalate and mono(2-ethyl-5-carboxypentyl) phthalate. After transformation to their tert-butyldimethylsilyl derivatives, they were analyzed by gas chromatography/mass spectrometry in the electron impact ionization mode. The calibration curves for the metabolites were linear at urinary concentrations of up to 30 μg/L, showing that they could be determined accurately and precisely (detection limits 0.1-0.4 μg/L, quantification limits 0.3-1.3 μg/L). The urine samples collected could be stored for up to 1 month at -20°C. The proposed analytical method was used to examine urine samples from seven healthy volunteers. This method should be useful for monitoring phthalate exposure in the general population.

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Simultaneous determination of some phthalate metabolites, parabens and benzophenone-3 in urine by ultra high pressure liquid chromatography tandem mass spectrometry

Cited by 85 publications

References 50 publications

Determination and separation of bisphenol A, phthalate metabolites and structural isomers of parabens in human urine with conventional high-pressure liquid chromatography combined with electrospray ionisation tandem mass spectrometry

Determination and separation of bisphenol A, phthalate metabolites and structural isomers of parabens in human urine with conventional high-pressure liquid chromatography combined with electrospray ionisation tandem mass spectrometry

A novel UPLC‐MS/MS method for sensitive quantitation of boldine in plasma, a potential anti‐inflammatory agent: application to a pharmacokinetic study in rats

Analytical method for urinary metabolites as biomarkers for monitoring exposure to phthalates by gas chromatography/mass spectrometry

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