Crystallization Process of Avermectin meal and impurity analysis.docVIP

 PAGE \* MERGEFORMAT 20 Crystallization Process of Avermectin meal and impurity analysis Author: Liu Ji Qing-Rong CHANG Zhi-dong, XIE Zhi-Feng Xing-Hua Sun Lei Zhang Guifeng Shen Shu-chao LIU Hui-zhou Keywords: Avermectin;, high-performance liquid chromatography;, MS;, impurities;, crystallization Abstract: Using high performance liquid chromatography (HPLC) electrospray ionization tandem mass spectrometry (ESIMSMS) method of the avermectin meal in the qualitative analysis of impurities. Identified the main impurity as: B1a structure similar B1b, A1a, A1b, A2a, A2b, B2a 6 Ge component, which A1a, B1b, B2a repeated crystallization is not easy to remove. Then examined the avermectin meal in methanol, ethanol, butanol and acetone in the re-crystallization, methanol and butanol for better removal of impurities; ethanol and acetone are equivalent, but the selective removal of different impurities. Keywords: Avermectin; high-performance liquid chromatography; mass spectrometry; impurities; crystallization Study on the crystallization of avermectin crude powder and its impurities analysis ABSTRACT Avermectin crude powder were purified by crystallization and its impurities were identified by HPLC (high performance liquid chromatography) ESIMSMS (electrospraymass spectrometrymass spectrometry). Main impurities in crude powder were B1b, A1a, A1b, A2a, A2b and B2a, which were similar to B1a in structure. The separation of A1a, B1b and B2a was very difficult due to their greatly similar structures to B1a. Recrystallizaton using methanol, ethanol, nbutanol and acetone as solvents were done respectively and it was found that methanol and nbutanol were good solvents for the separation of impurities. The impurities could be selectively separated using methanol or acetone. KEY WORDS Avermectin; HPLC; Mass spectrometry; Impurities; Crystallization Avermectin is a 16 yuan macrolide antibiotics, has a strong insecticidal acti