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LAAN-A-LC-E275$








            Application                  Supercritical Fluid Extraction / Chromatography

            News                         Application of Online SFE-SFC-PDA for Cleaning

                                         Validation
            No.L499$




            Cleaning validation is a process step that is extremely   Q Analytical Column Selection
            important for ensuring high quality and safety at   For SFC analysis, selection of the optimal column for the
            pharmaceutical manufacturing sites. Cloth used for   sample has a substantial effect on analysis reliability. We
            surface wiping, called a swab, is used to wipe a given   performed SFC separation of alkylbenzenesulfonate in four
            part of a piece of manufacturing equipment, and    different columns under the conditions shown in Table 1
            analysis of the wiped area of the swab is performed by   and Fig. 1, and chose the Shim-pack UCX-SIL analytical
            using high-performance liquid chromatography (HPLC)   column as it had the best peak shape. Based on an
            or a total organic carbon analysis (TOC). Evaluations   investigation of gradient profiles, we also found a relatively
            using HPLC have been increasingly used in recent years   steep gradient profile is suitable for quantitative analysis as
            because HPLC enables determination of individual   the properties of alkylbenzenesulfonate, which have
            compounds. Prior to analysis, an extraction procedure   different length of carbon chains, mean the significant
            must be performed on the swab. Using supercritical   peak broadiening if the gradient slope is not steep. Based
            fluid extraction (SFE) as the pretreatment method allows   on this information, we optimized analytical conditions
            for simple and quick target component extraction.   using the Shim-pack USX-SIL column and performed online
            Using supercritical fluid chromatography (SFC) after SFE   SFE-SFC analysis of a sample from a swab.
            also means that analysis results can be obtained simply
            by preparing the sample for SFE, which unifies the work
            flow from pretreatment to analysis. Please see
            Application News L496 for an overview of online SFE-
            SFC. This article describes the process of column
            selection using the Nexera-UC Chiral Screening System
            as the first step in analysis of the target compound
            alkylbenzenesulfonate.

                                         Table 1  SFC Analytical Conditions for Column Selection
                             Column    : Shim-pack UCX series columns (250 mm L. × 4.6 mm I.D., 5 μm)
                                         (i) UCX-RP (ODS with polar group), (ii) UCX-GIS (ODS), (iii) UCX-SIL, (iv) UCX-DIOL
                             Mobile Phase  : A: CO2; B: Methanol
                             Time Program  : Shown in the figure
                             Flowrate   : 3.0 mL/min
                             Column Temp. : 40 °C
                             Back Pressure  : 15 MPa
                             Wavelength   : 220 nm
                             Injection Vol.  : Shown in figure

                                                                                  Injected sample:
                                                                                    1 μL of 1 % standard sample

























                          Fig. 1  Comparison of SFC Separation of Standard Alkylbenzenesulfonate in Four Different Columns
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