Page 41 - Pharmaceutical Solution for Pharma Analysis
P. 41

Application  No.L499$
    News


            Q Online SFE-SFC Analysis of a Swab Containing
              Alkylbenzenesulfonate                                 uV (× 1,000,000)
            We investigated column selection by the scouting     3.0
            system, chose the Shim-pack UCX-SIL analytical column,   2.5  100 ng of alkylbenzenesulfonate
            optimized each analytical condition for online SFE-SFC
            analysis, then performed analysis using the conditions   2.0
            shown in Table 2 below.
                                                                 1.5                                    1st
                  Table 2  Analytical Conditions for Online SFE-SFC
                                                                 1.0                                    2nd
             [Sample Preparation]                                                                       3rd
             A total of 10 to 500 μg standard samples in methanol were dropped   0.5                    4th
             onto swabs.
             The swabs were enclosed into an extraction vessel and set to the SFE unit.  0.0
             [Static Extraction]                                     4.0  5.0  6.0  7.0  8.0  9.0  10.0 11.0  min
             Extraction Time : 3 min
             Mobile Phase  : A: CO2; B: 0.1 % (w/v) Ammonium Formate in Methanol
             B Conc.   : 10 %                                      Fig. 3  Confirmation of Online SFE Extraction Efficiency
             Flowrate   : 3.0 mL/min
             Back Pressure  : 15 MPa
             [Dynamic Extraction]
             Extraction Time : 3 min
             Mobile Phase  : A: CO2; B: Methanol                mAU
             B Conc.   : 10 %                                         Static  Dynamic     SFC
             Flowrate   : 3.0 mL/min                             3.0  Extraction  Extraction  Analysis
             Back Pressure  : 15 MPa
             [SFC]                                               2.5
             Column   : Shim-pack UCX-SIL (250 mm L. × 4.6 mm I.D., 5 μm)  Alkylbenzenesulfonate
             Mobile Phase  : A: CO2; B: Methanol                 2.0
             Time Program  :   10 %B (0-2 min), 10-60 %B (2-7 min),
                       60 %B (7-9 min), 10 %B (9-13 min)         1.5
             Flowrate   : 3.0 mL/min                                                                   500 μg
             Column Temp.  : 40 °C                                                                     200 μg
             Back Pressure  : 15 MPa                             1.0
             Wavelength   : 220 nm                                                                     100 μg
                                                                 0.5                                   50 μg
                                                                                                       20 μg
            The peak for the surfactant alkylbenzenesulfonate was   0                                  10 μg
            well-separated and detected as shown in Fig. 2 below.    -5.0  -2.5  0.0   2.5   5.0  7.5 min
            Fig. 3 shows the results of performing repeated SFE-SFC
            analyses from the same swab to which had been added
            an equivalent of 100 ng of alkylbenzenesulfonate. Since
            there was almost no alkylbenzenesulfonate peak evident
            from the second and later sample extractions, the
            extraction procedure was almost entirely complete after
            the first SFE. Fig. 4 shows the results of adding amounts
            of alkylbenzenesulfonate to swabs in the range of 10 to
            500 μg, and checking linearity. Within this range, the
            coefficient of determination that represents linearity was
            0.996. Fig. 5 shows the result of five consecutive
            analyses of separate swabs to which were added 100 μg
            of alkylbenzenesulfonate. Considering the process     Fig. 4  Linearity of Online SFE-SFC Analysis Using a Swab
            including extraction, the repeatability of retention times
            was 0.19 %RSD, and repeatability of peak area was
            5.76 %RSD. Based on these results, we confirmed the
            usefulness of the Nexera-US Online SFE-SFC System in   mAU
                                                                       Static
                                                                                              SFC
                                                                             Dynamic
            this application.                                     2.0  Extraction  Extraction  Analysis
                                                                       Alkylbenzenesulfonate
                                                                  1.5
                  200 μg of alkylbenzenesulfonate added in swab
                                                                  1.0
                    Swab blank                                    0.5


                                                                   0
                                                                      -5.5  -2.5   0.0   2.5    5.0   7.5 min
                                                                 Fig. 5  Repeatability of Online SFE-SFC Analysis Using a Swab
                -5.0   -2.5    0     2.5    5.0    7.5 min
               Fig. 2  Online SFE-SFC Analysis of Alkylbenzenesulfonate  Note: 6ZDE VDPSOHV ZHUH SURYLGHG E\ '$,,&+, 6$1.<2 &203$1<  /,0,7('
                                                                                                     6HFRQG Edition: )HE. 2016
                                                                                                     First Edition: Jan. 2016

                                               For Research Use Only. Not for use in diagnostic procedures.
                                               The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu.
                                               The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its
                                               accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the
                                               use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject
                                               to change without notice.
       www.shimadzu.com/an/                                                                        © Shimadzu Corporation, 2016
   36   37   38   39   40   41   42   43   44   45   46