HPLC Analysis of Cinacalcet Hydrochloride Impurities with a Purospher® STAR Phenyl Column
Materials
analytical column
mobile phase component
Milli-Q® IQ 7003/05/10/15 Ultrapure and Pure Water Purification Systems
Produces ultrapure (Type 1) water and pure (Type 2) water with a production flow rate of 3 L/hr from tap water feedCONDITIONS
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))
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 trademark of Merck KGaA, Darmstadt, Germany
Purospher is a registered trademark of Merck KGaA, Darmstadt, Germany