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制备型反相液相色谱法与逆流色谱法在百克级粗旋体杀虫剂纯化中的比较。

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

机构信息

Dow AgroSciences LLC, 9330 Zionsville Road, Indianapolis, IN 46268, USA.

出版信息

J Chromatogr A. 2011 Sep 9;1218(36):6122-7. doi: 10.1016/j.chroma.2011.06.073. Epub 2011 Jun 28.

DOI:10.1016/j.chroma.2011.06.073
PMID:21763662
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.

摘要

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。

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