Separation of perindopril tert-butylamine and(±)-1"epi-perindopril by high performance liquid chromatography
Objective:To develop an HPLC method for the separation of perindopril tert-butylamine and its epi-mer[(±)-1"-epi-perindopril tert-butylamine]and the determination of the epimer.Methods:Perindopril and(±)-1"-epi-perindopril were separated on an Agilent Poroshell CS-C18 column(100 mm × 3.0 mm,2.7 μm)maintained at 50 ℃ with the mobile phase containing a mixture of 0.15％sodium heptanesulfonate solution(adjusted to pH 2.0 with phosphoric acid)and acetonitrile-pentanol(217∶3)(82∶18,V/V)at 0.8 mL·min-1,and the detection wavelength was set at 215 nm.The injection volume was 2 μL.Results:(±)-1"-epi-perindopril and perindopril were separated successfully in 25 min with peak to valley ratio more than 3.0 or a resolution factor of 1.7.Good linear relationships were established between the peak response and the concentration in the range of 2-2 000 μg·mL-1 for the epimer and perindopril tert-butyl-amine(r＞0.999).The quantitative limits(S/N=10)were both about 1.0 μg·mL-1,and the detection limits(S/N=3)were both 0.3 μg·mL-1.The spiked recovery of the epimerer was 97.2％(RSD=1.8％,n=9).The content of(±)-1"-epi-perindopril tert-butylamine in 10 batches of samples ranged from 0.025％to 0.078％.Conclusion:The proposed method enhances the resolution efficiency,shows high accuracy,repeatabili-ty and stability.It can be effectively employed for the quality control of perindopril tert-butylamine.
perindopril tert-butylamine(±)-1"epi-perindopriltert-butylamineepimerHPLCstereoiso-mer separationimpurity determinationquality control
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