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Liquid Chromatograph Triple Quadrupole

            Liquid Chromatograph Mass Spectrometer (LCMS)                                                                             Mass Spectrometer (LC/MS/MS)






            Triglycerides                                                                                                             The application of GC/MS following derivatization with phenylboronic acid (DGF Standard methods 2009, Section C - Fats) has
                                                                                                                                      traditionally been used for analysis of 3-MCPD fatty acid esters, yet direct analysis by LC/MS/MS without derivatization is gaining attention
            DART (Direct Analysis in Real Time), when used with a mass spectrometer, permits quick analysis of analyte compounds without the need for   as an attractive alternative method. Significant amounts of 3-MCPD fatty acid esters are present in numerous natural vegetable oils, and
            sample pre-treatment. Generally, LC and GC are used for triglyceride analysis, but these methods are known to have such drawbacks as   their concentration is particularly high in palm oil. Shown here is the quantitative analysis of 3-MCPD fatty acid esters in palm oil using
            complicated sample preparation, long analysis time and carryover. Presented here is an analysis of lipids in food containing triglycerides,   LC/MS/MS.
            without conducting any sample using the LCMS-2020 equipped with DART as the ion source.
                                                                                                                                      Analytical Conditions
            The mass spectra of food product oils and fats (shortening and lard) with known fatty acid composition are shown as below. The
            monoglycerides, diglycerides and triglycerides were detected in the positive ion mass spectra of both samples. As for the negative ions,   Column   :Shim-pack XR-ODS II (75 mmL. × 2.0 mmI.D., 2.2 µm)
            linoleic acid and oleic acid were primarily detected in the shortening, while oleic acid was primarily detected in the lard.  Mobile phase A   :Methanol with 3 mmol/L Ammonium acetate / Acetonitrile = 9/1
                                                                                                                                      Mobile phase B   :Acetone / Methanol with 3 mmol/L Ammonium acetate / Acetonitrile = 8/1/1
                                                                                                                                      Time program    :0%B (0-2.5 min)     65%B (7.5 min)     100%B (7.51-10 min)     0%B (10.01-15 min)
            Analytical Conditions                                                                                                     Flow rate       :0.4 mL/min
                                                                                                                                      Injection volume   :2 µ
            DART heater temperature :400˚C                                                                                            Column temperature    :40°C
            Scan type       :m/z 50-1500 (Positive / Negative)                                                                        Probe voltage   :4.5 kV (ESI-Positive mode)
            Nebulizing gas flow   :1.5 L/min.                                                                                         Nebulizing gas flow    :1.5 L/min
            Drying gas flow   :5.0 L/min.                                                                                             DL temperature   :300°C
            DL temperature   :250˚C                                                                                                   Block heater temperature  :400°C
            Block heater temperature :400˚C                                                                                           DL / Q-array voltage   :Using default values
                                                                                                                                      Drying gas flow    :20 L/min





















                                                                                                                                                     MRM Chromatograms of the Synthetic Samples (1 µg/L, A:3-MCPD-Dipalmitoyl Ester,B: 3-MCPD-Dioleoyl Ester)




                            Mass Spectra for Shortening                         Mass Spectra for lard
            Reference: Application News C109 Application of Direct Analysis in Real Time (Part 2): Rapid Analysis of Triglycerides and Fatty Acids in Food Oil Using LCMS-2020


            Shimadzu Liquid Chromatograph Mass Spectrometer Product Lineup

                      Model                                            Features

                                      · Small footprint
                                      · UFscanning: 15,000 µ/sec high-speed scanning
                                      · UFswitching: 15 milliseconds high-speed polarity ionization switching time
                                      · UFsensitivity: High-speed analysis with high sensitivity
                                      · Robust, durable solution for difficult matrices and easy maintenance                                                                Calibration Curves (1-1000 µg/L,n=6)

                  LCMS-2020
                                                                                                                                      Reference: Application News C84 - Analysis of 3-MCPD Fatty Acid Diesters in Palm Oil using a Triple Quadrupole LC/MS/MS [LCMS-8030]

                                                                                                                                                                   Solutions for Palm Oil Analysis Application Notebook
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