Enantiospecific gas chromatographic—mass spectrometric procedure for the determination of ketoprofen and ibuprofen in synovial fluid and plasma: application to protein binding studies

Jack, Damon S.; Rumble, Roger; Davies, Noel W.; Francis, Hilton

doi:10.1016/0378-4347(92)80575-b

Cited by 19 publications

(13 citation statements)

References 20 publications

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“…Prior methods of analysis of ibuprofen have included HPLC, GC, and GC-MS [8][9][10][11][12][13][14][15]. Previously described HPLC and GC methods claim linearity to maximums ranging from 40-100 mg/L (8,(11)(12)(13)(14).…”

Section: Discussionmentioning

confidence: 99%

“…This time is longer but not unacceptable compared to an estimated 13 min per sample analyzed by HPLC (8,12). A previously published GC-MS method required two centrifugation steps and the timed, sequential addition of reagents to form first a mixed anhydride and next, an amine (10). Both this and another GC-MS method (9) used deuterated ibuprofen that was prepared on site.…”

Section: Discussionmentioning

confidence: 99%

“…Ibufenac (8,15) is not commercially available and is no longer supplied by the manufacturer for research. Other internal standards include naphthalene [14], 5-ethyl-5-p-tolylbarbituric acid (11), flurbiprofen (12), and deuterated ibuprofen (9,10). Use of flurbiprofen as an internal standard in the method presented here has the advantage of close chemical relationship to ibuprofen and ready commercial availability.…”

Section: Discussionmentioning

confidence: 99%

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Measurement of plasma ibuprofen by gas chromatography-mass spectrometry

Way

Wilhite

Smith

et al. 1997

J. Clin. Lab. Anal.

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A gas‐chromatography‐mass spectrometry (GC‐MS) method for the determination of plasma ibuprofen was developed. Plasma samples from cystic fibrosis (CF) patients receiving high‐dose ibuprofen therapy were analyzed by GC‐MS and the result compared to analysis by high‐performance liquid chromatography (reference method). Analysis of ibuprofen was sensitive to at least 5 mg/L, and the method was linear to 200 mg/L. Within‐run variations of plasma samples were 4.6% (131.7 ± 6.0 mg/L) and 5.4% (44.4 ± 2.4 mg/L), respectively. The between‐run variation was 9.3% (45.4 ± 4.2 mg/L) and 7.4% (88.0 ± 6.5 mg/L). This method is suited for routine clinical use for the monitoring of plasma ibuprofen levels in treatment of CF. It may be particularly applicable in pediatric laboratories, which are likely to possess GC‐MS capability. J. Clin. Lab. Anal. 11:336–339, 1997. © 1997 Wiley‐Liss, Inc.

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Section: Discussionmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

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Measurement of plasma ibuprofen by gas chromatography-mass spectrometry

Way

Wilhite

Smith

et al. 1997

J. Clin. Lab. Anal.

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“…Gas chromatography-mass spectrometry (Jack and Rumble, 1992), electrochromatography (Mayer and Shurig, 1993), capillary electrophoresis (Soini et al, 1994;Bjornsdottir et al, 1998), and nuclear magnetic resonance (Fulwood and Parker, 1992) have also been utilized as potential analytical techniques in enantiomeric separation of ibuprofen. These methods have proven to be less useful due to their inability to achieve baseline resolutions or their inability to removed the free acid of ibuprofen after separation.…”

Section: Other 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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“…In general terms, it is important to know both their whole concentration and their enantiomeric fraction in pharmaceuticals to prevent toxic or ineffective treatments. Several indirect chiral separation methods of PRO enantiomers have been reported in the literature [14][15][16] but direct methods based on the use of a chiral stationary phase (CSP) have been preferred [17]. The use of CSPs requires very clean samples before enantiomer chromatographic separation to keep the chiral column clean preventing its deterioration and enlarging its lifetime, which is an important factor due to the high cost of these columns.…”

Section: Introductionmentioning

confidence: 99%

Determination of profens in pharmaceuticals by heart‐cut achiral‐chiral two‐dimensional HPLC

Peñín-Ibáñez

Santos-Delgado

Polo-Díez

2018

Separation Science Plus

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Profens are important non‐steroidal anti‐inflammatory pharmaceutical drugs and their behavior depends on their enantiomeric form. Three of the most employed profens, ketoprofen, naproxen and ibuprofen, were separated simultaneously in pairs by two‐dimensional achiral‐chiral high‐performance liquid chromatography using heart‐cut mode. The total amount of each profen was determined using a C8 column in the first achiral system; in the second chiral system, the enantiomeric fraction of each profen was determined using an α1‐acid glycoprotein column. Mobile phases were optimized by factorial design, response surfaces and multi‐response analysis paying particular attention to mobile phase compatibility of both columns and to transferring time between systems. The effect of temperature on each profen and their enantiomer retention was studied, the thermodynamic parameters being calculated. Calibration graphs were linear in the ranges of 2–20, 0.5–10 and 10–40 mg/L for ketoprofen, naproxen and ibuprofen respectively in both systems. The method allowed the analysis of three pharmaceuticals establishing the enantiomeric fraction of each profen using a simple sample preparation; moreover, the first achiral system cleans the sample deeply preventing deterioration of the expensive chiral column. Recoveries over 80% and the enantiomeric fraction of each profen were obtained allowing determination of the pharmaceutical purity.

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Enantiospecific gas chromatographic—mass spectrometric procedure for the determination of ketoprofen and ibuprofen in synovial fluid and plasma: application to protein binding studies

Cited by 19 publications

References 20 publications

Measurement of plasma ibuprofen by gas chromatography-mass spectrometry

Measurement of plasma ibuprofen by gas chromatography-mass spectrometry

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

Determination of profens in pharmaceuticals by heart‐cut achiral‐chiral two‐dimensional HPLC

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