HPLC method validation and pharmacokinetic study of alendronate sodium in human urine with fluorescence detection

Hyun Suk Kang, Sung Joo Hwang, Jeong Sook Park, Chong Kook Kim

Research output: Contribution to journalArticle

14 Citations (Scopus)

Abstract

The purpose of this study was to validate a reliable analytical method for the pharmacokinetic study of alendronate sodium in human urine by a high performance liquid chromatography (HPLC) system with fluorescence detection. Alendronate sodium was extracted by using diethylamine (DEA) solid phase extraction (SPE) and derivatized with 9-fluorenylmethyl chloroformate (FMOC). Pamidronate was used as the internal standard. The sample was precipitated with sodium hydroxide and derivatized with FMOC in sodium carbonate buffer at pH 11.9. Separation was performed on a Capcell Pak UG C18 column (4.6mm x 150mm, 5 μm particles), using a gradient method starting with mobile phase acetonitrile/methanol-citrate/pyrophosphate buffer (28:72, v/v). The fluorometric detector was operated at 260 nm (excitation) and 310 nm (emission). The intra- and inter-day precision expressed as the relative standard deviation was less than 15%. The limit of quantification was 25 ng/mL of alendronate sodium using 5 mL of urine. The calibration curve was linear in the concentration range of 25-5000 ng/mL (r2 = 0.9999). Following the oral administration of 70 mg alendronate to volunteers, the cumulative amount of alendronate excreted (Aet) and peak excretion rate (Umax) were 198.39 ± 81.16 μg and 65.67 ± 20.83 μg/mL, respectively. The method was demonstrated to be highly feasible and reproducible for pharmacokinetic studies of alendronate sodium in seven volunteers after oral administration (70 mg as alendronate).

Original languageEnglish
Pages (from-to)1589-1600
Number of pages12
JournalJournal of Liquid Chromatography and Related Technologies
Volume29
Issue number11
DOIs
Publication statusPublished - 2006 Jul 1

Fingerprint

Alendronate
Pharmacokinetics
Validation Studies
High performance liquid chromatography
Fluorescence
High Pressure Liquid Chromatography
Urine
pamidronate
Oral Administration
Volunteers
Buffers
Sodium Hydroxide
Gradient methods
Solid Phase Extraction
Citric Acid
Calibration
Methanol
Detectors

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry
  • Biochemistry
  • Pharmaceutical Science
  • Clinical Biochemistry

Cite this

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abstract = "The purpose of this study was to validate a reliable analytical method for the pharmacokinetic study of alendronate sodium in human urine by a high performance liquid chromatography (HPLC) system with fluorescence detection. Alendronate sodium was extracted by using diethylamine (DEA) solid phase extraction (SPE) and derivatized with 9-fluorenylmethyl chloroformate (FMOC). Pamidronate was used as the internal standard. The sample was precipitated with sodium hydroxide and derivatized with FMOC in sodium carbonate buffer at pH 11.9. Separation was performed on a Capcell Pak UG C18 column (4.6mm x 150mm, 5 μm particles), using a gradient method starting with mobile phase acetonitrile/methanol-citrate/pyrophosphate buffer (28:72, v/v). The fluorometric detector was operated at 260 nm (excitation) and 310 nm (emission). The intra- and inter-day precision expressed as the relative standard deviation was less than 15{\%}. The limit of quantification was 25 ng/mL of alendronate sodium using 5 mL of urine. The calibration curve was linear in the concentration range of 25-5000 ng/mL (r2 = 0.9999). Following the oral administration of 70 mg alendronate to volunteers, the cumulative amount of alendronate excreted (Aet) and peak excretion rate (Umax) were 198.39 ± 81.16 μg and 65.67 ± 20.83 μg/mL, respectively. The method was demonstrated to be highly feasible and reproducible for pharmacokinetic studies of alendronate sodium in seven volunteers after oral administration (70 mg as alendronate).",
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HPLC method validation and pharmacokinetic study of alendronate sodium in human urine with fluorescence detection. / Kang, Hyun Suk; Hwang, Sung Joo; Park, Jeong Sook; Kim, Chong Kook.

In: Journal of Liquid Chromatography and Related Technologies, Vol. 29, No. 11, 01.07.2006, p. 1589-1600.

Research output: Contribution to journalArticle

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