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CHROMATOGRAPHY


generally easier to powderise, typically providing better quality results when used in drug screening and pharmacokinetic studies. All eluted compounds are finally collected in a highly volatile organic solvent, which reduces fraction dry- down time by up to 90% compared to conventional LC fractions.


PREPARATIVE PURIFICATION OF IBUPROFEN AND ITS ANALOGS Ibuprofen is one type of nonsteroidal anti-inflammatory drug (NSAID) used as a fever-reducing drug and analgesic. Te United States Pharmacopeia (USP) provides analytical methods for ibuprofen and its analog 4-isobutylacetophenone, using valerophenone as an internal standard.[2]


Fig. 2. Separate PFOS and PFOA to baseline in a fast, <2 min analysis (4.5 min total cycle time)


Tis article describes preparative


purification of these three components using the Shimadzu UFPLC system. Preparative LC and purification conditions are displayed in Table 1. Fig. 4 shows the preparative LC


chromatogram of the mixed solution of Ibuprofen and related compounds. It was prepared by dissolving the three target compounds with mobile phases to a concentration of 5,000 mg/L.


VERIFICATION OF PURITY OF IBUPROFEN AND ITS ANALOGS Te fractions of ibuprofen, valerophenone and 4-isobutylacetophenone collected by UFPLC were analysed by standard HPLC to verify the purity of the compounds. Table 2 shows the analytical conditions and Fig. 5 shows the chromatograms obtained for each fraction. Purities of the target compounds contained in each


Fig. 3. Chemical structures of Ibuprofen and related compounds


Fig. 4. Preparative LC chromatogram of Ibuprofen and its analogs (UFPLC)


fraction determined by area normalisation at UV 230 are listed in Table 3.


Fig. 5. HPLC analysis of Ibuprofen and related compounds in fractions obtained by UFPLC


ABOVE: Table 2. Conditions of analytical HPLC separation of purified fractions


BELOW: Table 3. Purities of target compounds contained in collected fractions (area percentage, UV 230 nm)


CONCLUSION Prominence UFPLC was shown to enable fast recovery of highly purified target compounds in a simple automated workflow. Ultra-high weight purity compounds can be obtained by implementing preparative separations and fraction purification. For powderisation of the pure sample, an extremely long drying time is necessary using conventional reversed-phase preparative LC, due to a high amount of water in the mobile phase. Moreover, in cases where a nonvolatile buffer solution is used, the salt can precipitate after drying. In preparative purification using UFPLC, it is possible to remove the nonvolatile salt used in the separation process, as desalting is performed in the trapping columns. Drying time is substantially reduced by use of organic solvent for sample recovery from the trapping columns, contributing greatly to improved efficiency in any application requiring preparative purification.


References: [1] N. Kosuke, Shimadzu Application News No. L526, Preparative Purification of Ibuprofen and Its Related Substances by Prominence UFPLC [2] USP Monograph for Ibuprofen


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