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Application   No. G296
    News



            „  Instrument Configuration and Analysis           „  Analysis of Diacetyl Derivatives Obtained Using
               Conditions                                         Shinwa DS-DA
            Table 1 lists the configuration of the instrument used for   After derivatizing diacetyl, the peak from DMQX was
            analysis and the analysis conditions.              detected in  the vicinity of a retention time of 9.6 min
                                                               (Fig. 4).
              Table 1  Instrument Configuration and Analysis Conditions   The dotted line in Fig. 5 indicates the calibration curve of a
             Gas chromatograph  : GC-2010 Plus                 15 % ethanol solution which was prepared in accordance
             Autosampler        : AOC-20i                      with the composition  of Japanese  sake  and then  added
             Sample injection port   :  SPL
             Column             : ULBON HR-52                  diacetyl. The  solid  line  is the calibration curve of  a
                                 (25 m × 0.25 mm I.D. df = 0.25 mm)  commercially available  sake which was added diacetyl.
             Detector           :  Flame ionization detector (FID)  From this we  were able to  determine  that  the  diacetyl
             Injection volume   :  2 μL                        content in  this  commercially available sake is  125 ppb
             Carrier gas        :  He, 30 cm/sec
             Split ratio        :  5:1                         (μg/L).
             Injection port temperature   :  200 °C
             Detector temperature   :  280 °C
             Column temperature   :  100 °C (2 min) - 10 °C/min -
                                 270 °C (5 min)









                                                     Diacetyl
                                                    derivative
                                                     DMQX






                                0           5.0         10.0         15.0         20.0  min
                                      Chromatogram of Japanese Sake Sample After Diacetyl Derivatization

                          1
                              Solid line: Commercially available sake
                        Peak area ratio [DMQX / internal standard substance]
                                  (contains diacetyl) with diacetyl added  y = 0.0016x + 0.2065
                              Dotted line: Dummy sake                R² = 0.9999
                         0.8      (contains no diacetyl) with diacetyl added



                         0.6
                                                                              y = 0.0016x + 0.0056
                                                                                  R² = 0.9997
                         0.4



                         0.2



                          0
                            0     50     100    150   200    250    300    350    400   450    500
                                                     Diacetyl concentration / ppb
                                              Calibration Curve of Diacetyl Derivative Sample
                                                                                                      First Edition: Oct. 2017
                                             For Research Use Only. Not for use in diagnostic procedure.
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