Determination of diclofenac sodium, flufenamic acid, indomethacin and ketoprofen by LC-APCI-MS.
A sensitive, selective and accurate high-performance liquid chromatography-mass spectrometry (LC-MS) assay for the determination of selected non-steroidal anti-inflammatory drugs (NSAIDs), namely diclofenac sodium (DIC), flufenamic acid (FLU), indomethacin (IND) and ketoprofen (KET), either individually or in mixtures, was developed. The examined drugs were injected onto Shim-pack GLC-CN column and were eluted with a mobile phase consisting of acetonitrile and 20 mM ammonium acetate solution (5:1 v/v)/pH 7.4 at a flow rate l ml min(-1). The mass spectrometer, operated in the single ion monitoring mode, was programmed to admit the negative ions [M-H] at m/z 295.9 (DIC), 280.1 (FLU), 355.8 (IND) and 252.9 (KET), respectively. The calibration curves were linear (r > or = 0.9993) over the concentration range 50-300 ng ml(-1) (FLU, DIC) and 100-500 ng ml(-1) (KET, IND) with detection limits of 0.5-4.0 ng. The mean predicted concentrations for the analytes were in the range -5.9 and 5.2% of the nominal concentrations. Within-day and between-day precision were in the range of 0.8-9.1% of the R.S.D. Mean recovery percentages of the individual compounds from laboratory-made mixtures and pharmaceutical formulations were (99.5-101.5%) and (100.6-102.2%), respectively.
Abdel-Hamid
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ME
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Health Science Center, Kuwait University, Kuwait. abdel-hamid@hsc.kuniv.edu.kw
Novotny
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L
Hamza
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H
D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis*; D002214:Capsules / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004008:Diclofenac / Q000032:analysis*; D005439:Flufenamic Acid / Q000032:analysis*; D007213:Indomethacin / Q000032:analysis*; D007660:Ketoprofen / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D012680:Sensitivity and Specificity; D013607:Tablets / Q000737:chemistry
D000894:Anti-Inflammatory Agents, Non-Steroidal; D002214:Capsules; D013607:Tablets; D004008:Diclofenac; D005439:Flufenamic Acid; D007660:Ketoprofen; D007213:Indomethacin