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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
Ethyl Acetate, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Flurbiprofen, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Ethyl acetate
Sigma-Aldrich
Ethyl acetate
Sigma-Aldrich
Ultrapure Acetonitrile
Supelco
Methylene Chloride, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
Flurbiprofen, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Dichloromethane, suitable for HPLC, ≥99.8%, contains amylene as stabilizer
Sigma-Aldrich
Acetonitrile, suitable for HPLC-GC, ≥99.8% (GC)
Sigma-Aldrich
Dichloromethane, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.9%, contains 50-150 ppm amylene as stabilizer
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Acetonitrile, ≥99.9% (GC)
Sigma-Aldrich
Ethyl acetate, suitable for HPLC, ≥99.7%
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Acetonitrile, HPLC Plus, ≥99.9%
Sigma-Aldrich
Ethyl acetate, HPLC Plus, for HPLC, GC, and residue analysis, 99.9%
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Ethyl acetate, suitable for HPLC, ≥99.8%
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Hexane, suitable for HPLC, ≥97.0% (GC)
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Hexane, HPLC Plus, for HPLC, GC, and residue analysis, ≥95%
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Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
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Hexane, suitable for HPLC, ≥95%
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Dichloromethane, ACS reagent, ≥99.5%, contains 40-150 ppm amylene as stabilizer
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Acetonitrile, ReagentPlus®, 99%
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Hexane, ReagentPlus®, ≥99%
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Ethyl acetate, ACS reagent, ≥99.5%
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Dichloromethane, contains 40-150 ppm amylene as stabilizer, ACS reagent, ≥99.5%
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Hexane, Laboratory Reagent, ≥95%
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Acetonitrile, ≥99.8% (GC)
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Hexane, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥99% (GC)
Sigma-Aldrich
Dichloromethane, puriss., meets analytical specification of Ph. Eur., NF, ≥99% (GC)