Determination of urinary ortho- and meta-cresol in humans by headspace SPME gas chromatography/mass spectrometry

Fustinoni, Silvia; Mercadante, Rosa; Campo, Laura; Scibetta, Licia; Valla, C.; Foà, V.

doi:10.1016/j.jchromb.2004.12.029

Cited by 24 publications

(32 citation statements)

References 27 publications

(39 reference statements)

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“…Ortho-cresol main working solution was prepared in acetonitrile obtained from Merck® (Darmstadt, Germany), to the concentration of 5 mg/L. For the SPME tests, according to Fustinoni et al [14], sodium chloride and sodium hydroxide were purchased from Vetec® (Rio de Janeiro, Brazil), hydrochloric acid; ethyl acetate and acetic acid were obtained from Dinâmica® (São Paulo, Brazil). Sample preparation for SPE required the use of potassium monobasic phosphate, ethyl acetate obtained from Vetec® (Rio de Janeiro, Brazil), methanol obtained from Synth® (São Paulo, Brazil), acetic acid, hexane and methylene chloride obtained from Dinâmica® (São Paulo, Brazil).…”

Section: Chemical Reagentsmentioning

confidence: 99%

See 1 more Smart Citation

New Gas Chromatographic/Mass Spectrometric Method for Ortho-Cresol Detection in Urine

Frohlich¹,

Sebben²,

Ferraz³

2017

JBBD

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Section: Chemical Reagentsmentioning

confidence: 99%

“…Analytical conditions were based on Fustinoni et al [14]: Injection port temperature and transfer line temperature were set to 250°C. Helium (He) 6.0 (99.9999%) was used as carrier gas at 1 mL/min in constant flow with the injection port operating in splitless mode.…”

Section: Chromatographical Conditions: Gc/msmentioning

confidence: 99%

New Gas Chromatographic/Mass Spectrometric Method for Ortho-Cresol Detection in Urine

Frohlich¹,

Sebben²,

Ferraz³

2017

JBBD

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“…The use was not limited to occupational health where the method was originally developed [1][2][3][4][5][6] , but also in environmental health fields 7,8) . The method has been applied to analysis for un-metabolized mother chemicals 1,[9][10][11][12] as well as for metabolites after proper automated derivatization of metabolites to increase volatility [13][14][15][16] .…”

Section: Introductionmentioning

confidence: 99%

Use of a Holder-vacuum Tube Device to Save On-site Hands in Preparing Urine Samples for Head-space Gas-chromatography, and Its Application to Determine the Time Allowance for Sample Sealing

et al. 2011

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To facilitate urine sample preparation prior to head-space gas-chromatographic (HS-GC) analysis. Urine samples containing one of the five solvents (acetone, methanol, methyl ethyl ketone, methyl isobutyl ketone and toluene) at the levels of biological exposure limits were aspirated into a vacuum tube via holder, a device commercially available for venous blood collection (the vacuum tube method). The urine sample, 5 ml, was quantitatively transferred to a 20-ml head-space vial prior to HS-GC analysis. The loaded tubes were stored at +4°C in dark for up to 3 d. The vacuum tube method facilitated on-site procedures of urine sample preparation for HS-GC with no significant loss of solvents in the sample and no need of skilled hands, whereas on-site sample preparation time was significantly reduced. Furthermore, no loss of solvents was detected during the 3-d storage, irrespective of hydrophilic (acetone) or lipophilic solvent (toluene). In a pilot application, high performance of the vacuum tube method in sealing a sample in an air-tight space succeeded to confirm that no solvent will be lost when sealing is completed within 5 min after urine voiding, and that the allowance time is as long as 30 min in case of toluene in urine. The use of the holder-vacuum tube device not only saves hands for transfer of the sample to air-tight space, but facilitates sample storage prior to HS-GC analysis.

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“…[14][15][16] Since only about 1.0% of the absorbed toluene is transformed into cresols, 9,17 more sensitive techniques are necessary for their determination such as gas or highperformance liquid chromatography generally coupled to a mass detector. 1,18 Irrespective of the identification technique, previous sample preparation is required starting with the hydrolysis of urinary conjugates, followed by liquid-liquid extraction, 8,17 C18 19 or vapor stream distillation. 1 Solid-phase microextraction (SPME) is an extraction technique introduced by C. Arthur and J. Pawliszyn in 1990, 20 and is a rapid, simple and sensitive extraction method for the analysis of aqueous samples.…”

Section: Introductionmentioning

confidence: 99%

“…23,24 This extraction technique has many advantages such as the fact that no solvents are used, easy handling, relatively short extraction time, direct injection of the analytes into the gas chromatograph, and good linearity for many substances. SPME has been used for the determination of volatile and semivolatile compounds present in water, 22,25 and biological material, 18,[26][27][28] among others. 29 In the present study, we describe an analytical method for the determination of o-cresol in urine using SPME by direct immersion of the fiber in the biological material, after acid hydrolysis of the conjugates, followed by capillary gas chromatography-flame ionization detection.…”

Section: Introductionmentioning

confidence: 99%

Analysis of ortho-cresol in urine by solid phase microextraction-capillary gas chromatography

Paiva

Martins²,

Siqueira³

2007

J. Braz. Chem. Soc.

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Neste trabalho foi desenvolvido um método usando a microextração em fase sólida (SPME) para análise cromatográfica em fase gasosa capilar com detector de ionização por chama (CG/ IC) de orto-cresol urinário, metabólito do tolueno. Após otimização das variáveis da SPME e da validação do método, foram analisadas amostras de urina de 27 trabalhadores expostos a solventes em oficinas de reparo automotivo. As melhores condições de extração foram obtidas com a hidrólise ácida da urina, extração em fibra de carbowax/divinilbenzeno (CW/DVB) 70 μm por 20 min em pH neutro, com adição de 3 g de Na 2 SO 4 , sob agitação. O método mostrou linearidade entre 0,1 e 1,5 mg L -1 de o-cresol em urina, LOQ de 0,1 mg L -1 , repetibilidade entre 6,8 e 7,8%. O valor médio de o-cresol em urina dos trabalhadores foi de 0,35 ± 0,23 mg L -1 . O método SPME/CG/DIC mostrou ser rápido, simples e aplicável para fins de biomonitorização de trabalhadores expostos.The object of the present study was the development of method for the determination of urinary ortho-cresol using solid-phase microextraction (SPME), followed by capillary gas chromatography-flame ionization detection (GC/FID). After optimization of the SPME variables and validation of the method, it was applied to analysis of o-cresol in urine collected from 27 workers exposed to solvents in automotive repair shops. The maximum extraction efficiency was obtained using fiber of carbowax-divinylbenzene (CW/DVB), 70 μm, immerged 20 min in acid hydrolysed urine added with 3 g Na 2 SO 4 at pH 7.0 and under magnetic stirring. The method showed linearity between 0.1 to 1.5 mg L -1 , LOQ of 0.1 mg L -1 , precision between 6.8 to 7.8% CV. Mean o-cresol in urine from exposed workers was 0.35 ± 0.23 mg L -1 . The SPME-GC/FID method is fast, simple and can be applied to the occupational toluene biomonitoring.

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Determination of urinary ortho- and meta-cresol in humans by headspace SPME gas chromatography/mass spectrometry

Cited by 24 publications

References 27 publications

New Gas Chromatographic/Mass Spectrometric Method for Ortho-Cresol Detection in Urine

New Gas Chromatographic/Mass Spectrometric Method for Ortho-Cresol Detection in Urine

Use of a Holder-vacuum Tube Device to Save On-site Hands in Preparing Urine Samples for Head-space Gas-chromatography, and Its Application to Determine the Time Allowance for Sample Sealing

Analysis of ortho-cresol in urine by solid phase microextraction-capillary gas chromatography

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