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CHROMATOGRAPHY


harmaceutical companies are developing compounds of increased complexity – drugs with numerous functional groups in a single molecule, polymeric compounds, biopharmaceuticals such as peptides, proteins and many others – that must be purified, in production quantities. Regulatory agencies continue to press for more stringent requirements in purity of pharmaceutical products and, especially, drug substances. An acute need exists for other tools in addition to crystallisation, the classic technique for purification, to address a growing number of purification problems. Currently, preparative HPLC is the


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most powerful and versatile method for purification tasks in the pharmaceutical industry. Te Prominence ultra-fast preparative and purification liquid chromatograph (UFPLC) enables substantial labour savings in preparative purification.


Tis happens by automation not only of fractionation of the target compound but also the related processes of concentration, purification and recovery. Tis article introduces an example of preparative purification of a mixed sample of the pharmaceutical compound ibuprofen and its analogs using Shimadzu’s UFPLC Advanced System (Fig. 1).[1] UFPLC automatically performs


the various processes related to preparative isolation of target compounds using a combination of preparative LC and trapping columns. Details of these processes are as follows: separation of target


Fig. 1. Prominence UFPLC


PURIFICATION MADE EASY


Preparative purification of ibuprofen and its related substances by UFPLC


Table 1. Conditions of preparative LC separation and purification by UFPLC system


compounds in complex sample by preparative LC and introduction into trapping columns; replacement of solvent in trapping columns with ultrapure water; and elution of target compounds from trapping columns by organic solvent. An outline of the respective processes is shown in Fig. 2.


Te system integrates preparative LC with fraction trapping for up to five compounds of interest. It is controlled by a dedicated walk-up software designed to simplify the workflow also for non-expert users. It allows users to easily set conditions for chromatographic separation and isolation of target compounds, trapping, eluting and collecting highly purified compounds in as little as 90


22 www.scientistlive.com


minutes. For applications involving the isolation of low concentration targets, replicate injection and collection to the same trapping column to increase the amount of compound trapped on column prior to elution is easily accomplished.


HIGH PURITY COMPOUNDS, OPTIONALLY RECOVERED AS A FREE BASE Te Prominence UFPLC eliminates some of the problems associated with conventional prep LC, especially poor purity of collected compounds due to mobile phase additives, which become contaminants in the final collected fraction and inhibit powderisation. Shimadzu’s Shim-pack C2P-H trapping column strongly retains target compounds, allowing unwanted organic solvents, water and additives to be flushed away. Additionally, rinsing the column with an aqueous ammonia solution after trapping allows compounds to be recovered as free bases which are


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