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Application   No. C153
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                       Table 4  Quantitative Results of the               Table 5  Quantitative Results of the
                       Manual Pretreatment Method and                     Manual Pretreatment Method and
                  Fully Automated Pretreatment Analysis Method       Fully Automated Pretreatment Analysis Method
                              (Amiodarone)                                    (Desethylamiodarone)
                                   Amiodarone                                       Desethylamiodarone
                            Manual    Automated                                Manual  Automated   Ratio %*
                            [ng/mL]   [ng/mL]   Ratio %*                       [ng/mL]   [ng/mL]
                   Sample 1   373     411      110.2                  Sample 1  304      271      89.1
                   Sample 2   399     404      101.3                  Sample 2  412      366      88.8
                   Sample 3   546     557      102.0                  Sample 3  416      423      101.7
                   Sample 4   205     211      102.9                  Sample 4  271      240      88.6
                   Sample 5   963     895      92.9                   Sample 5  717      654      91.2
                   Sample 6   1,318   1,213    92.0                   Sample 6  151      150      99.3
                   Sample 7   1,271   1,229    96.7                   Sample 7  431      408      94.7
                   Sample 8   1,233   1,282    104.0                  Sample 8  664      628      94.6
                   Sample 9   2,259   2,208    97.7                   Sample 9  940      1,080    114.9
                   Average                     100.0                  Average                     95.9
                   RSD %                        5.8                   RSD %                        8.9

                        * Automated Pretreatment / Manual Pretreatment     * Automated Pretreatment / Manual Pretreatment

                                 AMD                                                 DEA
                  2500            R² = 0.9946                        1250            R² = 0.9541
                                                                                     y = 1.007x
                                   y = 0.975x
               Automated Pretreatment  [ng/mL]  1500              Automated Pretreatment  [ng/mL]  750
                  2000
                                                                     1000
                                                                     500
                  1000
                  500
                                                                     250
                    0
                                                                                     500
                                                                                            750
                           500
                      0
                                  1000
                                        1500
                               Manual Pretreatment  2000  2500         0  0    250  Manual Pretreatment  1000  1250
                                    [ng/mL]                                            [ng/mL]

                   Comparison of Quantitative Results for Amiodarone        Comparison of Quantitative Results
                                                                             for Desethylamiodarone

                                  Table 6  Analysis Conditions (Comparative Test of Pretreatment Methods)
                        System       : CLAM-2000 + Nexera + LCMS-8040
                        Protocol     : Plasma disp. 50 μL - acetonitrile disp. 225 μL - mixing at 1900 rpm, 120 sec - filtration for 90 sec
                        Column       : Shimadzu GLC Mastro C18 (50 mmL. × 2.1 mmI.D., 3 μm)
                        Mobile Phase   : A) 0.1% Formic acid - Water, B) 0.1% Formic acid - Methanol
                        Flow Rate    : 0.4 mL/min
                        Time program   : B Conc. 10 % (0 min) – 100 % (2 – 3.5 min) – 10 % (3.51 – 6 min)
                        Column Temp.   50 °C                Injection Volume  : 0.1 μL
                        Probe Voltage   : 4.5 kV (ESI-positive mode)
                        DL Temp.     : 250 °C               Block Heater Temp.  : 400 °C
                        Neb. Gas Flow   : 3 L/min           Drying Gas Flow  : 15 L/min

            [Acknowledgments]
            We would like to thank pharmacist Yuko Shimamoto of the Pharmacy Division at the National Cerebral and Cardiovascular Center Hospital
            (National Research and Development Agency) in Japan for her significant cooperation in the investigation provided in this article.

            References  •  Guidance for Industry : Bioanalytical Method Validation (2001, US FDA)
                     •  Guideline on Bioanalytical Method Validation in Pharmaceutical Development (2013, Japan MHLW)

            Notes    •  The product described in this document has not been approved or certified as a medical device under the Pharmaceutical and
                      Medical Device Act of Japan. It cannot be used for the purpose of medical examination and treatment or related procedures.
                     •  The samples described in this  document were all sampled  and measured  at the National  Cerebral and Cardiovascular  Center
                      Hospital in Japan. Permission was obtained regarding the publication of measurement data.




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