ABSTRACT
Objective:To establish an HPLC method compatible with the mass spectrometry for the determination of the content and related substances in amlodipine besylate tablets. Methods:The sample was separated on a CAPCELL PAK C18 column (250 mm × 4. 6 mm, 5 μm) with the mobile phase consisting of methanol and 20 mmol·L-1 ammonium acetate (60∶40) at a flow rate of 1. 0 ml·min-1 . The detection wavelength was set at 237 nm. The column temperature was 35℃ and the injection volume was 20 μl. Be-sides, an HPLC-QTOF MS method was used to identify the molecular structure of the related substances of amlodipine. Results: The related substances were completely separated from amlodipine. The linear range of amlodipine besylate was 10-100 μg · ml-1 ( r =0. 999 8), and the mean recovery was 99. 2%(RSD=1. 0%,n=9). The main related substances could be detected by HPLC-QTOF MS. Conclusion:The established method is accurate, reliable and reproducible, which can be used in the quality control of amlodip-ine besylate tablets.
ABSTRACT
AIM: To establish the method for determination of gentiopicrin, palmatine hydrochloride and berberine hydrochloride in Ertong Ⅱ Oral Liquid (Cortex Phellodendri, Radix Gentianae, Rhizoma Anemarrhenae, etc.) by RP HPLC. METHODS: The column was a Diamonsil TM C 18 column (250mm?4.6mm, 5?m); the mobile phase was CH 3CN H 3PO 4 C 6H 15 N H 2O; The ultraviolet detection was set at 270nm; the flow rate was 1mL?min -1 . RESULTS: The linear ranges of gentiopicrin, palmatine hydrochloride and berberine hydrochloride were 72.8～728?g?mL -1 ( r=0.9998 ), 7.55～75.5?g?mL -1 ( r=0.9998 ), 12.45～124.5?g?mL -1 ( r = 0.9999 ), respectively. The average recoveries ( n =6) of gentiopicrin, palmatine hydrochloride and berberine hydrochloride were 98.17%, 98.78%, 98.60%; RSD were 1.60%, 1.35%, 1.25%, respectively. CONCLUSION: The method is accurate, reproducible and highly selective, thus suitable for quality control of Er Tong Ⅱ Oral Liqual.