APP501

HPLC Analysis of Cinacalcet Hydrochloride Impurities with a Purospher^® STAR Phenyl Column

Properties

• technique(s): HPLC: suitable
• test parameters: column: Purospher^® STAR Phenyl (5 µm) LiChroCART^® 150 x 4.6 mm I.D. (1.51922); mobile phase: [A] 10 mmol/L Sodium perchlorate solution, adjusted to pH 2.5 with perchloric acid; [B] Acetonitrile; gradient: 0-0.5 min 2.5% B, in 4.5 min to 95%B, 2 min 95%B, 3 min at 2.5%B; flow rate: 1.0 mL/min; pressure: 60 bar (870 psi); column temp.: 60°C (Sampler: 10 °C); detector: UV, 215 nm (analytical flow cell; 10 µL); injection: 5 µL; sample/matrix: Impurity identification solution with cinacalcet impurities A, B, C at 1.5 µg/mL each and cinacalcet at 5 µg/mL in solvnt mixture (10 mmol/L sodium perchlorate solution, adjusted to pH 2.5 with perchloric acid, and acetonitrile in a ratio of 50:50 (%v/v))
• application(s): pharmaceutical

Description

General description

Cinacalcet hydrochloride is an oral calcimimetic indicated for the treatment of secondary hyperthyroidism in patients on dialysis with end-stage renal disease, and in patients with parathyroid carcinoma to reduce hypercalcemia.

Analysis Note

The developed method on a Purospher^® STAR Phenyl, 150 × 4.6 mm (5µm) column was found to be linear for cinacalcet hydrochloride up to a concentration of 6 µg/mL with a LOQ of 0.65 µg/mL and LOD of 0.21 µg/mL. For cinacalcet impurity A, impurity B and impurity C, the method was linear up to a concentration of 1.8 µg/mL with LOQ ranging from 0.03 to 0.13 µg/mL and LOD ranging from 0.01 to 0.04 µg/mL. The method can be applied for the study of related substances in cinacalcet hydrochloride API using the Purospher^® STAR Phenyl HPLC column. Repeatability for the cinacalcet 5 µg/mL solution was 1.19% RSD (n=5). The tailing factor for cinacalcet eluting at 12.3 min was NMT 2.0 (1.31) and the theoretical plate count was significantly above 2000.

Other Notes

App_501

Legal Information

LICHROCART is a registered trademark of Merck KGaA, Darmstadt, Germany

Purospher is a registered trademark of Merck KGaA, Darmstadt, Germany