Dow AgroSciences LLC, 9330 Zionsville Road, Indianapolis, IN 46268, USA.
J Chromatogr A. 2011 Sep 9;1218(36):6122-7. doi: 10.1016/j.chroma.2011.06.073. Epub 2011 Jun 28.
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.
反相高效液相色谱 (RP-HPLC) 和高效逆流色谱 (HPCCC) 被用于两种半合成多杀菌素,spinetoram-J 和 spinetoram-L 的中试规模纯化,这两种化合物是商业杀虫剂 spinetoram 的主要成分。对两个独立进行的 1 公斤级别的纯化实验进行了比较。两种方法都以纯度>97%的方式获得了这两种成分,spinetoram-J 和 spinetoram-L 的收率分别超过了 93%和理论值的 63%。HPCCC 工艺的通量比制备规模的 RP-HPLC 高 2 倍,消耗的溶剂约少 70%,HPCCC 产物的馏分体积仅为 HPLC 的 7%,因此需要的后处理步骤更少。