Assay of naproxen by high-performance liquid chromatography and identification of its photoproducts by LC-ESI MS

Abstract

A rapid, accurate and reliable reversed-phase high-performance liquid chromatographic (HPLC) method for the determination of naproxen and its photodegradation products in methanol was developed and validated. An Inertsil 5-ODS-3V column (5 microm, C18, 250 x 4.6 mm i.d.) was used with a mobile phase of acetonitrile-methanol-1% HOAc in H2O (40:20:40, v/v/v). UV detection was set at 230 nm. The developed method satisfies system suitability criteria, peak integrity and resolution for the parent drug and its photoproducts. The intraday and interday standard deviations of five replicate determinations for five consecutive days at the working concentrations of 5.0, 10, 25, 50, and 100 microm were 0.23-0.98 with coefficients of variance (CVs) of between 0.96 and 4.56% for the former, and 0.14-1.15 with CVs of between 1.13 and 3.82% for the latter. The percentage recoveries were determined to be 98.34, 99.19, 100.18, 102.97 and 99.81%, respectively, at the five concentrations between 5.0 and 100 microm. The limit of quantitation of naproxen was determined to be 0.29 microg/mL, while the detection limit was 64 ng/mL. Four major photoproducts were observed from the HPLC chromatogram using a Panchum PR-2000 reactor which equipped with 8 W x 16 low-pressure quartz mercury lamps as the light source for irradiation of a naproxen sample in methanol. The structures of the photoproducts were confirmed by LC-ESI MS.

Development and Validation of Liquid Chromatography- Mass Spectroscopy/Mass Spectroscopy Method for Quantitative Analysis of Naproxen in Human Plasma after Liquid-Liquid Extraction

“…Most of its therapeutic activity is probably mediated through prostaglandin synthesis inhibition [6][7][8]. Several chromatographic methods have been reported for determination of naproxen in raw material [9], tablets [10][11][12], plasma [13][14][15], urine [16], intestinal perfusion samples [17] and pharmaceutical preparations [18][19][20].…”

A Validated Stability-Indicating UHPLC Method for Determination of Naproxen and Its Related Compounds in Bulk Drug Samples

“…Naproxen is cited in the European Pharmacopoeia to have contamination by compounds A, B, D, E [5,6] and Imp-C is likely to be present in the preparation of Naproxen by using asymmetric hydrogenation step process [7]. A survey on literature reveals that many chromatographic methods have been reported for the determination of Naproxen in raw material [8], tablets [9,10], plasma [11][12][13], urine [14], intestinal perfusion samples [15] and pharmaceutical preparations [16]. However, no stability indicating UHPLC method is reported for estimation of related compounds and assay of naproxen from bulk drug samples.…”

Spectrophotometric determination of Naproxen as ion-pair with bromophenol blue in bulk, pharmaceutical preparation and human serum samples

“…Naproxen is rapidly and completely absorbed after oral administration, and it is the predominant species in serum, with a therapeutic range of 30 to 90 μg mL -1 4 . Naproxen has been determined by several analytical methods like: HPLC [5][6][7] , HPTLC 8 , LC-MS/MS 9,10 , capillary electrophoresis 11,12 , fluorimetric methods 13 , chemiluminescence [14][15][16] , voltammetry 17,18 , solid-phase microextraction coupled with liquid chromatography 19 and spectrophotometry [20][21][22] . Although the HPLC methods are highly sensitive and specific, but they are most expensive.…”