Solid-phase microextraction for the determination of the free concentration of valproic acid in human plasma by capillary gas chromatography

Krogh, Mette; Johansen, Karianne; Tønnesen, Finn; Rasmussen, Knut

doi:10.1016/0378-4347(95)00273-8

Cited by 72 publications

(42 citation statements)

References 27 publications

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“…-Recovery describes the extraction efficiency of the analytical process. Recovery was calculated by comparing the peak areas of analytes obtained from the SPE processed blank saliva sample previously spiked with analytes vs. peak areas obtained from an SPE processed blank saliva sample, and then spiked with analytes, representing 100 % recovery (15).…”

Section: Bioanalytical Methods Validationmentioning

confidence: 99%

Development and validation of a bioanalytical LC-UV method with solid-phase extraction for determination of valproic acid in saliva

Tonic-Ribarska¹,

Haxhiu²,

Sterjev³

et al. 2012

Acta Pharmaceutica

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Valproic acid (2-propylpentanoic acid) is an anticonvulsant drug, widely used in the treatment of epilepsy, affecting both children and adults (1, 2). It is also used to treat bipolar disorder and to prevent migraine headaches (3).Therapeutic drug monitoring (TDM) of antiepileptic drugs (AEDs) is used in clinical practice to aid the treatment of patients with epilepsy. In order to obtain information A bioanalytical HPLC method with UV detection for the determination of the antiepileptic drug valproic acid in human saliva has been developed and validated. Saliva represents an alternative matrix for therapeutic monitoring of antiepileptic drugs due to the increasing interest in free drug concentration. The proposed method involved solid-phase extraction for sample preparation and yielded very good mean recoveries of 99.4 % and 97.9 % for valproic acid and IS, respectively. The calibration function for valproic acid was linear over the concentration range of 1.0-50.0 mg mL -1 (R 2 = 0.9989). Within-run and between-run precision and accuracy were studied at four concentrations and RSDs were less than 7.3 and 2.2 %, while accuracy values were higher than 96.8 and 97.5 %, respectively. The described method provides sensitivity, linearity, precision, accuracy and is suitable for analyses of valproic acid in saliva samples.

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Section: Bioanalytical Methods Validationmentioning

confidence: 99%

Development and validation of a bioanalytical LC-UV method with solid-phase extraction for determination of valproic acid in saliva

Tonic-Ribarska¹,

Haxhiu²,

Sterjev³

et al. 2012

Acta Pharmaceutica

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show abstract

“…Gas chromatography (GC), [3][4][5][6][7][8][9] liquid chromatography [10][11][12][13][14][15][16][17][18][19][20] and capillary electrophoresis [21][22][23] are the main reported techniques for the determination of VPA.…”

Section: Introductionmentioning

confidence: 99%

Headspace Solid-Phase Microextraction-Gas Chromatography Method for the Determination of Valproic Acid in Human Serum, and Formulations Using Hollow-Fiber Coated Wire

et al. 2009

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“…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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Solid-phase microextraction for the determination of the free concentration of valproic acid in human plasma by capillary gas chromatography

Cited by 72 publications

References 27 publications

Development and validation of a bioanalytical LC-UV method with solid-phase extraction for determination of valproic acid in saliva

Development and validation of a bioanalytical LC-UV method with solid-phase extraction for determination of valproic acid in saliva

Headspace Solid-Phase Microextraction-Gas Chromatography Method for the Determination of Valproic Acid in Human Serum, and Formulations Using Hollow-Fiber Coated Wire

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

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