Objective: To establish an HPLC method for simultaneous determination of three isomers in captopril API and tablets. Methods: A Chiralpak IG chiral column (250 mm×4.6 mm, 5 μm) was adopted. The mobile phase A was n-hexane-trifluoroacetic acid (100∶0.1) and the mobile phase B was anhydrous ethanol-trifluoroacetic acid (100∶0.1) with gradient elution. The flow rate was 1.0 mL·min-1. The temperature of the column was set at 35 ℃, and the wavelength was set at 215 nm. The injection volume was 10 μL. Results: The method had a good specificity,and no interferences from the excipients were found. Captopril and its three isomers were well separated. The average recoveries were 99.6%, 102.1% and 93.6%, with RSD of 1.7%, 1.4% and 2.0%, respectively. The RSD of repeatability were all less than 2.0%. The test solution was stable after 24 h. The quantification limits of diastereoisomer Ⅰ,enantiomer and impurity F were 0.91,0.99 and 3.23 μg·mL-1, respectively. The detection limits were 0.27, 0.30 and 0.97 μg·mL-1, respectively. The calibration curve showed good linearity over the range of 1.82-45.51 μg·mL-1 of diastereoisomer Ⅰ, 0.99-39.71 μg·mL-1 of enantiomer, 3.23-40.33 μg·mL-1 of impurity F (r was 0.999 0-1.000 0), respectively. The contents of impurity F in three batches of captopril were 0.04%,0.04% and 0.03%, respectively. The contents of impurity F in three batches of captopril tablets were 0.03%, 0.03% and 0.03%, respectively. No diastereoisomer Ⅰ or enantiomer were detected in captopril and tablets. Conclusion: The methodology validation results showed that the method is suitable for the determination of three isomers in captopril and tablets.
SHEN Yue, FAN Jia-li, LUO Gang, LI Jian-wei
. Determination of three isomers in captopril API and tablets by HPLC[J]. Chinese Journal of Pharmaceutical Analysis, 2023
, 43(3)
: 457
-462
.
DOI: 10.16155/j.0254-1793.2023.03.12
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