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  • Determination of flurbiprofen in human plasma by gas chromatography with mass spectrometry and its pharmacokinetics.

Determination of flurbiprofen in human plasma by gas chromatography with mass spectrometry and its pharmacokinetics.

Journal of AOAC International (2014-08-26)
Bilal Yilmaz, Huseyin Sahin, Vedat Akba, Ali Fuat Erdem
ABSTRACT

This paper describes a GCIMS method for the determination of flurbiprofen in human plasma. Flurbiprofen and internal standard ibuprofen were extracted from plasma by using a liquid-liquid extraction method. Derivatization was carried out using N-Methyl-N-(trimethylsilyl)trifluoroacetamide. The calibration curve was linear between the concentration range of 0.10 and 5.0 microg/mL. Intraday and interday precision values for flurbiprofen in plasma were less than 5.49%, and accuracy (relative error) was better than 5.33%. The extraction recoveries of flurbiprofen from human plasma were between 93.6 and 98.6%. The LOD and LOQ of flurbiprofen were 0.03 and 0.10 microg/mL, respectively. This assay was applied to determine the pharmacokinetic parameters of flurbiprofen in healthy Turkish volunteers who had been given 100 mg of flurbiprofen.

MATERIALS
Product Number
Brand
Product Description

Supelco
1-Butanol, analytical standard
Sigma-Aldrich
Chloroform, ≥99%, PCR Reagent, contains amylenes as stabilizer
Sigma-Aldrich
Ibuprofen, meets USP testing specifications
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1-Butanol, Molecular Biology, ≥99%
Supelco
N-Methyl-bis(trifluoroacetamide), derivatization grade (GC derivatization), LiChropur, ≥97.0% (GC)
Supelco
Chloroform, analytical standard
Sigma-Aldrich
Ibuprofen, ≥98% (GC)
Sigma-Aldrich
1-Butanol, anhydrous, 99.8%
Sigma-Aldrich
Chloroform, anhydrous, ≥99%, contains 0.5-1.0% ethanol as stabilizer
Sigma-Aldrich
Chloroform, anhydrous, contains amylenes as stabilizer, ≥99%
Supelco
N-Methyl-bis(trifluoroacetamide), derivatization grade (GC derivatization), LiChropur, ≥99.0% (GC)
Supelco
Ibuprofen, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Chloroform, contains ethanol as stabilizer, ACS reagent, ≥99.8%
Sigma-Aldrich
Chloroform, contains 100-200 ppm amylenes as stabilizer, ≥99.5%
Supelco
Ibuprofen
USP
Ibuprofen, United States Pharmacopeia (USP) Reference Standard
Ibuprofen for peak identification, European Pharmacopoeia (EP) Reference Standard
Ibuprofen, European Pharmacopoeia (EP) Reference Standard
Supelco
Acetonitrile(Neat), Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Residual Solvent - Acetonitrile(solution in DMSO), Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Chloroform, ACS spectrophotometric grade, ≥99.8%, contains 0.5-1.0% ethanol as stabilizer
Sigma-Aldrich
Chloroform, contains amylenes as stabilizer, ACS reagent, ≥99.8%
Sigma-Aldrich
1-Butanol, ACS reagent, ≥99.4%
Sigma-Aldrich
1-Butanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.5% (GC)
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1-Butanol, 99.9%
Supelco
1-Butanol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Chloroform, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
1-Butanol, suitable for HPLC, ≥99.7%
Supelco
Acetonitrile, analytical standard
Sigma-Aldrich
Acetic anhydride, ACS reagent, ≥98.0%