Stereospecific high-performance liquid chromatographic assay of ibuprofen: improved sensitivity and sample processing efficiency

Lemko, C.; Caillé, Gilles; Foster, Robert T.

doi:10.1016/0378-4347(93)80126-o

Cited by 46 publications

(23 citation statements)

References 17 publications

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“…More commonly, ibuprofen is derivatized with optically pure chiral amines e.g. L-leucinamide [30,31], (R)-and (S)-Iphenylethylamine [32,33], (R)-and (S)-amphetamine [34,35], (R)-and (S)-l-(naphthen-l-yl)ethylamine [36][37][38][39] and (-)-2-[4-(1-aminoethyl)phenyl]-6-methoxybenzoxazole [40]. The use of chiral amines with strong chromophores or fluorophores has the added advantage of enhancing detection.…”

Section: Introductionmentioning

confidence: 99%

Enantiospecific analysis of ibuprofen by high performance liquid chromatography: Determination of free and total drug enantiomer concentrations in serum and urine

et al. 1997

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SummaryA reversed-phase high-performance liquid chromatographic (HPLC) assay, based on the indirect approach to enantiomeric analysis, for the determination of ibuprofen in human serum and urine has been developed. Following the addition of (R,S)-flurbiprofen, as internal standard, the enantiomers of ibuprofen were isolated from plasma and urine samples by liquid-liquid extraction at acidic pH. The enantiomers of flurbiprofen and ibuprofen were derivatized with (R)-l-(naphthen-1-yl)ethylamine, using 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide and 1-hydroxybenzotriazole as coupling reagents, to yield the corresponding diastereoisomeric amides. Chromatographic resolution of the derivatives was achieved using a C18 column (Waters Resolve C18; 5 gin, 150 x 3.9 mm) using a mobile phase of phosphate buffer (pH 3.5, 0.01 M): acetonitrile (50:50 v/v) at a flow rate of 1.5 mL min -1 at ambient temperature. Quantification was carried out using a spectrofluorometer with excitation and emission wavelengths of 290 and 330 nm respectively. The use of a semimicrobore column (150 x 2.1 mm) containing the same stationary phase facilitated the analysis of the free drug enantiomer concentrations following equilibrium dialysis. The derivatization procedure was carried out as described above but with a reduction in the quantities of the reagents used in order to reduce the background noise in the chromatographic analysis. The HPLC methodology for the determination of free drug enantiomer concentrations was validated against a previously reported method employing the radiolabelled drug.

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Section: Introductionmentioning

confidence: 99%

Enantiospecific analysis of ibuprofen by high performance liquid chromatography: Determination of free and total drug enantiomer concentrations in serum and urine

et al. 1997

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“…Good separati on of target compounds and short run ti me were obtained using a mobile phase system of 20 mM phosphate buff er (pH 7) containing 0.1% TFA-acetonitrile (65:35, v/v). The retenti on ti me of ibuprofen (7.3 min) was quite short than that studied in other papers [6][7][8] . When this method is applied to plasma samples, its sensiti vity was found to be adequate for pharmacokineti c studies.…”

mentioning

confidence: 51%

Yüksek Performanslı Sıvı Kromatografisi Kullanarak Tavşan Plazmasında İbuprofenin Tayini

Yılmaz¹,

Aşçı²,

Palabıyık³

2009

Kafkas Univ Vet Fak Derg

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SummaryThe aim of the present study was to develop and validate a procedure based on high-performance liquid chromatography (HPLC) for determination of ibuprofen in rabbit plasma. Separation of ibuprofen and naproxen (internal standard, IS) was achieved on an Ace C18 column (5 μm, 250x4.6 mm i.d.) using UV detection with λ=225 nm. The mobile phase consisted of 20 mM phosphate buffer (pH 7) containing 0.1% trifluoroacetic acid (TFA)-acetonitrile (65:35, v/v). The analysis was performed in less than 10 min with a flow rate of 1 mL/min. Excellent linearity was found between 0.5 and 40 μg/mL. Intra-and inter-day precision values for ibuprofen in plasma were less than 4.97, and accuracy (relative error) was better than 7.20%. The recoveries for all samples were >92.8%. The limits of detection (LOD) and quantification (LOQ) of ibuprofen were 0.10 and 0.25 μg/mL, respectively. The described HPLC method has adequate sensitivity and specificity to study pharmacokinetics of ibuprofen in rabbits, and could be adapted also to clinical pharmacokinetic study.Keywords: Ibuprofen, HPLC, Liquid-liquid extraction, Rabbit, Pharmacokinetic study Yüksek Performanslı Sıvı Kromatografisi Kullanarak Tavşan Plazmasında İbuprofenin Tayini ÖzetBu çalışmanın amacı tavşan plazmasında ibuprofenin tespit edilmesi için yüksek basınçlı sıvı kromatografisine (YBSK) dayalı bir yöntem geliştirmek ve valide etmektir. İbuprofen ve naproksenin (internal standart, IS) ayırımı dalga boyu λ=225 nm olan UV dedektör kullanılarak C18 kolon (5 μm, 250x4.6 mm i.d.) ile yapılmıştır. Mobil faz %0.1 trifluoroasetik asit içeren 20 mM fosfat tamponu (pH 7)-asetonitril (65:35, h/h) den oluşmuştur. Analiz 1 mL/dk akış hızı ile 10 dakikadan daha az sürede yapılmıştır. 0.5 ve 40 μg/mL arasında çok iyi linearite bulunmuştur. Plazmada ibuprofen için gün içi ve günler arası kesinlik değerleri %4.97'den küçüktü, ve doğruluk (bağıl hata) %7.20'den daha iyiydi. Bütün örnekler için geri kazanım >%92.8 idi. İbuprofenin saptanabilen (LOD) ve ölçülebilen (LOQ) en düşük değeri sırasıyla 0.10 and 0.25 μg/mL'dir. Tanımlanan YBSK metodu tavşanlarda ibuprofenin farmakokinetiğini incelemek için yeterli duyarlılığa ve özgüllüğe sahiptir ve klinik farmakokinetik çalışmalara da uyarlanabilir.

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“…There are extensive reports in the literature concerning prederivatization techniques (Khoa et al, 1994;Griffith et al, 1993;Lemko et al, 1993;Wright et al, 1992;Toyo'oka et al, 1992). A chiral derivatization reagent that has an appropriate chromophore or fluorophore is a useful tool for analysis of ibuprofen with respect to selectivity, sensitivity, and versatility (Kondo et al, 1993;Toyo'oka et al, 1992).…”

Section: Chromatographic Separation Methodsmentioning

confidence: 99%

Review- Alternatives for the separation of drug enantiomers: ibuprofen as a model compound

Carvalho

Cass

Calafatti

et al. 2006

Braz. J. Chem. Eng.

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-Given the inherent dangers associated with racemic pharmaceuticals, exhaustive studies of techniques designed to separate enantiomers have been conducted. This paper reports a brief review of the different physical, chemical, and enzymatic methods used for the enantiomeric separation of rac-ibuprofen. The possible contribution of each technique to the preparation of enantiomerically pure drugs is reviewed in the context of competitive approaches that depend on the scale of application, with special emphasis on the recent progress achieved in this particular area.

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Stereospecific high-performance liquid chromatographic assay of ibuprofen: improved sensitivity and sample processing efficiency

Cited by 46 publications

References 17 publications

Enantiospecific analysis of ibuprofen by high performance liquid chromatography: Determination of free and total drug enantiomer concentrations in serum and urine

Enantiospecific analysis of ibuprofen by high performance liquid chromatography: Determination of free and total drug enantiomer concentrations in serum and urine

Yüksek Performanslı Sıvı Kromatografisi Kullanarak Tavşan Plazmasında İbuprofenin Tayini

Review- Alternatives for the separation of drug enantiomers: ibuprofen as a model compound

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