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

被引:51
作者
DeAmicis, Carl [1 ]
Edwards, Neil A. [2 ]
Giles, Michael B. [2 ]
Harris, Guy H. [3 ]
Hewitson, Peter [4 ]
Janaway, Lee [2 ]
Ignatova, Svetlana [4 ]
机构
[1] Dow AgroSci LLC, Indianapolis, IN 46268 USA
[2] Dynam Extract Ltd, Slough, Berks, England
[3] Dynam Extract Inc, Monmouth Jct, NJ 08852 USA
[4] Brunel Univ, Adv Bioproc Ctr, Uxbridge UB8 3PH, Middx, England
基金
英国生物技术与生命科学研究理事会;
关键词
Pilot scale; HPCCC; HPLC; Spinetoram; Spinosyns;
D O I
10.1016/j.chroma.2011.06.073
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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. (C) 2011 Elsevier B.V. All rights reserved.
引用
收藏
页码:6122 / 6127
页数:6
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