TY - JOUR
T1 - Structural elucidation of potential impurities in azilsartan bulk drug by HPLC
AU - Zhou, Wentao
AU - Zhou, Yuxia
AU - Sun, Lili
AU - Zou, Qiaogen
AU - Wei, Ping
AU - Ouyang, Pingkai
PY - 2014/11/1
Y1 - 2014/11/1
N2 - During the synthesis of Azilsartan (AZS), it was speculated that 15 potential impurities would arise. This study investigated the possible mechanism for the formation of 14 of them, and their structures were characterized and confirmed by IR, NMR, and MS techniques. In addition, an efficient chromatographic method was developed to separate and quantify these impurities, using an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm) in gradient mode with a mixture of acetonitrile and the potassium dihydrogen orthophosphate buffer (10 mM, pH adjusted to 3.0 with phosphoric acid). The HPLC method was validated for specificity, precision, accuracy, and sensitivity. LOQ of impurities were in the range of 1.04-2.20 ng. Correlation coefficient values of linearity were >0.9996 for AZS and its impurities. The mean recoveries of all impurities in AZS were between 93.0 and 109.7%. Thus, the validated HPLC method is suitable for the separation and quantification of all potential impurities in AZS.
AB - During the synthesis of Azilsartan (AZS), it was speculated that 15 potential impurities would arise. This study investigated the possible mechanism for the formation of 14 of them, and their structures were characterized and confirmed by IR, NMR, and MS techniques. In addition, an efficient chromatographic method was developed to separate and quantify these impurities, using an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm) in gradient mode with a mixture of acetonitrile and the potassium dihydrogen orthophosphate buffer (10 mM, pH adjusted to 3.0 with phosphoric acid). The HPLC method was validated for specificity, precision, accuracy, and sensitivity. LOQ of impurities were in the range of 1.04-2.20 ng. Correlation coefficient values of linearity were >0.9996 for AZS and its impurities. The mean recoveries of all impurities in AZS were between 93.0 and 109.7%. Thus, the validated HPLC method is suitable for the separation and quantification of all potential impurities in AZS.
UR - http://www.scopus.com/inward/record.url?scp=84915815050&partnerID=8YFLogxK
U2 - 10.5740/jaoacint.14-022
DO - 10.5740/jaoacint.14-022
M3 - 文章
C2 - 25632433
AN - SCOPUS:84915815050
SN - 1060-3271
VL - 97
SP - 1552
EP - 1562
JO - Journal of AOAC International
JF - Journal of AOAC International
IS - 6
ER -