Simultaneous Determination of Twelve Related Substances in Rosuvastatin Calcium Bulk Drug by HPLC

An HPLC method for the simultaneous determination of twelve related substances(2 - 13) in rosuvastatin calcium(1) was established. The Welch C18 column(4.6 mm×250 mm，5 µm) was used, and the analysis was carried out in the gradient elution mode, with a solvent mixture comprising of 1％ trifluoroacetic acid in water, acetonitrile and water(1∶35∶65, volume ratio) as mobile phase A, and a solvent mixture comprising of 1％trifluoroacetic acid in water, acetonitrile and water(1∶90∶10, volume ratio) as mobile phase B. The detection wavelength was 242 nm, the flow rate was 1.0 mL/min, and the column temperature was 40 ℃. The results showed that the resolution between 1 and its related substances was greater than 1.5, and it was linear for 1 - 13 in the corresponding mass concentration ranges. The LODs of 1 - 13 were 0.028 95 - 0.060 21 µg/mL, and the LOQs were 0.096 50 - 0.200 71 µg/mL. The average recoveries(n=9) of 2 - 13 were 94.59％ - 102.00％, with the RSDs of 0.79％ - 4.06％. The determination results of three batches of 1 bulk drug showed that the contents of all related substances were less than 0.1％ and the total impurity content was less than 1.0％, except related substance 3, whose content was less than 0.2％. The established method has good resolution, high sensitivity and specificity, which is suitable for the determination of related substances in 1. © 2023 Shanghai Institute of Pharmaceutical Industry. All rights reserved.