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

Yi Hsin Hsu, Yi B. Liou, Jen A. Lee, Chau Yang Chen, An-Bang Wu

Research output: Contribution to journalArticle

27 Citations (Scopus)

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 μm, C18, 250 × 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 μM 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 μM. The limit of quantitation of naproxen was determined to be 0.29 μg/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 × 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.

Original languageEnglish
Pages (from-to)787-793
Number of pages7
JournalBiomedical Chromatography
Volume20
Issue number8
DOIs
Publication statusPublished - Aug 2006

Fingerprint

Naproxen
High performance liquid chromatography
Methanol
Assays
High Pressure Liquid Chromatography
Mercury vapor lamps
Quartz
Photolysis
Photodegradation
Liquids
Mercury
Light sources
Limit of Detection
Irradiation
Light
Pressure
Recovery
Pharmaceutical Preparations

Keywords

  • HPLC
  • LC-ESI MS
  • Naproxen
  • Photoproducts
  • Validation

ASJC Scopus subject areas

  • Biochemistry, Genetics and Molecular Biology(all)
  • Biochemistry
  • Clinical Biochemistry
  • Analytical Chemistry
  • Pharmacology

Cite this

Assay of naproxen by high-performance liquid chromatography and identification of its photoproducts by LC-ESI MS. / Hsu, Yi Hsin; Liou, Yi B.; Lee, Jen A.; Chen, Chau Yang; Wu, An-Bang.

In: Biomedical Chromatography, Vol. 20, No. 8, 08.2006, p. 787-793.

Research output: Contribution to journalArticle

Hsu, Yi Hsin ; Liou, Yi B. ; Lee, Jen A. ; Chen, Chau Yang ; Wu, An-Bang. / Assay of naproxen by high-performance liquid chromatography and identification of its photoproducts by LC-ESI MS. In: Biomedical Chromatography. 2006 ; Vol. 20, No. 8. pp. 787-793.
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N2 - 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 μm, C18, 250 × 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 μM 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 μM. The limit of quantitation of naproxen was determined to be 0.29 μg/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 × 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.

AB - 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 μm, C18, 250 × 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 μM 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 μM. The limit of quantitation of naproxen was determined to be 0.29 μg/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 × 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.

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