Comparison of preparative reversed phase liquid chromatography and countercurrent chromatography for the kilogram scale purification of crude spinetoram insecticide

• Published in: Journal of Chromatography A Vol. 1218; no. 36; pp. 6122 - 6127
• Main Authors: DeAmicis, Carl, Edwards, Neil A., Giles, Michael B., Harris, Guy H., Hewitson, Peter, Janaway, Lee, Ignatova, Svetlana
• Format: Journal Article Conference Proceeding
• Language: English
• Published: Amsterdam Elsevier B.V 09.09.2011; Elsevier
• Subjects: Analytical chemistry; Biological and medical sciences; Chemical control; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - methods; Chromatography, Reverse-Phase - methods; Control; countercurrent chromatography; Countercurrent Distribution - methods; Exact sciences and technology; Fundamental and applied biological sciences. Psychology; HPCCC; HPLC; insecticides; Insecticides - isolation & purification; Macrolides - isolation & purification; Other chromatographic methods; Phytopathology. Animal pests. Plant and forest protection; Pilot scale; Protozoa. Invertebrates; reversed-phase high performance liquid chromatography; reversed-phase liquid chromatography; solvents; Spinetoram; Spinosyns; HPCCC; Spinosyns; Spinetoram; Pilot scale; HPLC; Countercurrent chromatography; Insecticide; Purification; Preparative chromatography; Pesticides; HPLC chromatography; Pilot plant scale; Polyketide; Reversed phase chromatography; Comparative study
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2011.06.073

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, 1kg, 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.