Published:Journal of Chromatographic Science, ISSN 0021-9665Volume 44, Number 4, April 2006, pp. 200-204

A Gradient HPLC Test Procedure for the Determination of Impurities and the Synthetic Precursors in 2-[4-(1-Hydroxy-4-[4-(Hydroxydiphenylmethyl)-1-Piperidinyl]-butyl)-Phenyl]-2-Methylpropionic Acid

C. B’Hymer
University of Cincinnati, Mail Location 0172, Cincinnati, OH 45221-0172

A gradient high-performance liquid chromatographic (HPLC) test procedure is developed and evaluated for its ability to establish the levels of impurities and remaining synthetic precursors in 2-[4-(1-hydroxy-4-[4-(hydroxydiphenylmethyl)-1-piperidinyl]-butyl)-phenyl]-2-methylpropionic acid. A gradient program with a mobile phase of 0.02M sodium phosphate buffer and 0.004M sodium perchlorate in acetonitrile–water (~ pH 2.5) is used with a Spherisorb C6 column. The acetonitrile composition is increased linearly from 40% to 65% over a 45-min period and held at 65% for 20 min. UV detection at 210 nm is used to quantitate all components. The procedure is validated for accuracy using spiked levels (0.1% to 1.5%, w/w) with two suspected impurities, the synthetic precursors. A multiday repeatability study using two different Spherisorb C6 columns and HPLC systems shows consistent impurity quantitation results with one production lot of the bulk compound.

Reproduction of editorial content of this journal is prohibited without publisher’s permission.

Site Map: Home | Current Issue | Subscribe | Back Issues | About Us | Meetings | Advertising |
| Books for Sale | For the Author | Links | Supplier Info | Search |