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Fast Analysis of 3-MCPD and 2-MCPD on Rxi-17Sil MS

GC_FS0569
PeakstR (min)Conc.
(ng/mL)
1.3-MCPD-d5 PBA derivative4.143100
2.3-MCPD PBA derivative4.169200
3.2-MCPD-d5 PBA derivative4.388100
4.2-MCPD PBA derivative4.418100
ColumnRxi-17Sil MS, 20 m, 0.18 mm ID, 0.18 µm (cat.# 14102)
Standard/SampleSee notes
Diluent:Isooctane
Injection
Inj. Vol.:1 µL PTV split (split ratio 10:1)
Liner:Topaz 2.0 mm ID straight inlet liner w/wool (cat.# 23314)
Inlet Temp. Program:120 °C to 165 °C at 300 °C/min (hold 10 min) to 320 °C at 300 °C/min (hold 8 min)
Oven
Oven Temp.:120 °C (hold 0.5 min) to 200 °C at 18.5 °C/min to 330 °C at 35 °C/min
Carrier GasHe, constant flow
Flow Rate:1 mL/min
DetectorMS
Mode:SIM
SIM Program:147, 150, 196, 201 m/z, 50 ms dwell
Transfer Line Temp.:320 °C
Analyzer Type:Quadrupole
Source Type:Inert
Source Temp.:230 °C
Quad Temp.:150 °C
Ionization Mode:EI
InstrumentAgilent 7890A GC & 5975C MSD
Sample PreparationStandards were derivatized with 20 µL phenylboronic acid (saturated solution in diethyl ether), dried, and then reconstituted in 1 mL isooctane. Final concentrations are given in the peak table.