Abstract
One unknown impurity in azoxystrobin bulk material at a level 0.15% was detected by a gradient reverse phase high performance liquid chromatography (HPLC). This impurity was isolated from a crude sample of azoxystrobin using reverse phase preparative LC. The impurity isolated by preparative LC was characterized by NMR, MS experimental data. Based on the results obtained from different spectroscopic experiments, these impurity was characterized as methyl 2-(2- (6- (2-cyanophenoxy)-2-((4-(2-cyanophenoxy)-6- (2- (1, 3-dimethoxy-3-oxoprop-l-en-2-yl)phenoxy) pyrimidin-5-yl) methyl)pyrimidin-4-yloxy)phenyl)-3-methoxyacrylate. Formation of this impurity is also discussed.
Highlights
Azoxystrobin, methyl 2-(2-(6-(2-cyanophenoxy)pyrimidin-4-yloxy)phenyl-3-methoxy acrylate is a potent antifungal agent1-3
The stringent purity requirement from regulatory agencies5 that all the individual impurity, which are ≥ 0.1%, must be identified and characterized, this paper aims at the identification and characterization of an unknown impurity in azoxystrobin active ingredient by LC-MS/MS and NMR4
The targeted impurity under study are marked as Impurity I eluted at retention times of about 23 min and azoxystrobin eluted at about 18 min
Summary
Azoxystrobin, methyl 2-(2-(6-(2-cyanophenoxy)pyrimidin-4-yloxy)phenyl-3-methoxy acrylate is a potent antifungal agent. High performance liquid chromatographic (HPLC) method was developed for testing of purity of azoxystrobin bulk material. The stringent purity requirement from regulatory agencies that all the individual impurity, which are ≥ 0.1%, must be identified and characterized, this paper aims at the identification and characterization of an unknown impurity in azoxystrobin active ingredient by LC-MS/MS and NMR4. To the best of our knowledge, this impurity is novel, and not reported in literature. Since the impurity level is low, after trying several days, failed to enrich the impurity level by synthetic route. A thorough study has been undertaken to develop a preparative LC method to isolate, wherever possible, and characterize this impurity by chromatographic and spectroscopic techniques
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