title: Comparison of preparative reversed phase liquid chromatography and countercurrent chromatography for the kilogram scale purification of crude spinetoram insecticide.
abstract: Reversed phase HPLC (RP-HPLC) and high performance countercurrent chromatography (HPCCC) were compared for the pilot scale purification of two semi-synthetic spinosyns, spinetoram-J and spinetoram-L, the major components of the commercial insecticide spinetoram. Two, independently performed, 1 kg, purification campaigns were compared. Each method resulted in the isolation of both components at a purity of >97% and yields for spinetoram-J and spinetoram-L of >93% and ≥ 63% of theoretical, respectively. The HPCCC process produced a 2-fold higher throughput and consumed approximately 70% less solvent than preparative scale RP-HPLC, the volume of product containing fractions from HPCCC amounted to 7% of that produced by HPLC and so required much less post-run processing.
authors.affiliation: Dow AgroSciences LLC, 9330 Zionsville Road, Indianapolis, IN 46268, USA. CVDeamicis@dow.com
authors.forename: Carl
authors.initials: C
authors.lastname: DeAmicis
authors.forename: Neil A
authors.initials: NA
authors.lastname: Edwards
authors.forename: Michael B
authors.initials: MB
authors.lastname: Giles
authors.forename: Guy H
authors.initials: GH
authors.lastname: Harris
authors.forename: Peter
authors.initials: P
authors.lastname: Hewitson
authors.forename: Lee
authors.initials: L
authors.lastname: Janaway
authors.forename: Svetlana
authors.initials: S
authors.lastname: Ignatova
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D056148:Chromatography, Reverse-Phase / Q000379:methods*; D003377:Countercurrent Distribution / Q000379:methods*; D007306:Insecticides / Q000302:isolation & purification*; D018942:Macrolides / Q000302:isolation & purification*
chemical_list: D007306:Insecticides; D018942:Macrolides; C548262:spinetoram