方案摘要
方案下载应用领域 | 制药/生物制药 |
检测样本 | 其他 |
检测项目 | 其他 |
参考标准 | 暂无 |
The purification of a valuable product or product library after a long and complex synthesis is a very important process. The Agilent Automated Purifi cation Software introduces an Open-Access-based solution for isolating substances, with automated focused gradient to simplify the pre- and post-purification steps. This Technical Overview describes the easy steps to follow, from crude sample analytical scouting submission to pure target product archiving or screening. For example, a purification sample containing a target peak overlapped by an impurity was purifi ed on the Agilent 1260 Infinity Preparative-Scale LC/MS Purifi cation System using the Automated Purifi cation Software. This purifi cation produced a pure target compound with 88 % recovery, saving 40 % of solvent and runtime compared to a standard purifi cation method.
Abstract
The purification of a valuable product or product library after a long and complex synthesis is a very important process. The Agilent Automated Purifi cation Software introduces an Open-Access-based solution for isolating substances, with automated focused gradient to simplify the pre- and post-purification steps.
This Technical Overview describes the easy steps to follow, from crude sample analytical scouting submission to pure target product archiving or screening. For example, a purification sample containing a target peak overlapped by an impurity was purifi ed on the Agilent 1260 Infinity Preparative-Scale LC/MS Purifi cation System using the Automated Purifi cation Software. This purifi cation produced a pure target compound with 88 % recovery, saving 40 % of solvent and runtime compared to a standard purifi cation method.
Introduction
In synthetic chemistry, automation of the purifi cation process is one of the keys for increasing the productivity of a research group. Scaling-up a compound separation performed on an analytical system to a preparative liquid chromatography system requires an optimization step on the analytical column. This step concerns the development of the gradient method for the isolation of the target compound with the best balance between purity, throughput, and time. For these perspectives, a focused gradient profi le offers the best solution for the purifi cation of the target compound. To enhance the fi ne focused gradient profi le, the user must have a good knowledge of preparative liquid chromatography and method development (more detail about the analytical to preparative scale-up process in the Agilent Technical Overview, 5991-2013EN1 ).
The Agilent Automated Purifi cation Software combines the performance of the focused gradients and automation of the preparative chromatography workfl ow. This add-on to the Agilent OpenLAB CDS Chemstation gives users privileges in an Open-Access work environment.
To that end, the software provides two different user modes:
• In the Expert Mode, users can easily choose to use the default automated purifi cation settings or use a customized method profi le.
• In the Easy-Prep mode, the operators follow the defined easy-to-use user interface.
The method used in the Easy-prep mode can only be fully managed and customized by the administrator.
This Technical Overview describes the purifi cation steps in the Easy-Prep mode, described from the simplifi ed operator view.
Conclusion
The Agilent Automated Purifi cation Software Add-On coupled with the Agilent OpenLAB CDS ChemStation Edition for LC and LC/MS Systems offers an automated solution to achieve higher throughput.
With an automated on-the-fl y gradient generation, based on the target mass or formula of the desired product, the chromatographic selectivity is increased on the automated identifi ed target peak. Thus, the optimized purifi cation method allows shorter run time and decreases the solvent consumption by 40 %.
Furthermore, with the Easy-prep mode of the Automated Purifi cation Software, preparative method development is no longer required, opening access of the purifi cation system to nonexpert users with diverse chromatographic experience.
This Technical Overview demonstrates how 54 mg of a targeted compound was purifi ed using the Agilent 1260 Infi nity Preparative-Scale LC/MS Purifi cation System, with 88 % recovery and 100 % purity.
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