Sugar TFA oximes on Rtx-1701

	Peaks	t_R (min)
1.	(E)-Fucose-TFA-oxime	2.048
2.	(E)-Ribose-TFA-oxime	2.132
3.	(E)-Arabinose-TFA-oxime	2.176
4.	(Z)-Ribose-TFA-oxime	2.320
5.	(Z)-Fucose-TFA-oxime	2.347
6.	(E)-Xylose-TFA-oxime	2.376

	Peaks	t_R (min)
7.	(Z)-Arabinose-TFA-oxime	2.473
8.	(Z)-Xylose-TFA-oxime	2.555
9.	(E)-Mannose-TFA-oxime	2.646
10.	(E)-Glucose-TFA-oxime	2.719
11.	(Z)-Mannose-TFA-oxime	2.830
12.	(Z)-Glucose-TFA-oxime	2.894

Injection
Column	Rtx-1701, 30 m, 0.25 mm ID, 0.25 µm (cat.# 12023)
Standard/Sample	Sugar TFA oximes
Diluent:	Ethyl acetate
Conc.:	1-5 mg of starting material
Inj. Vol.:	1 µL split (split ratio 100:1)
Liner:	Topaz 4.0 mm ID Precision Inlet Liner w/ Wool (cat.# 23305)
Inj. Temp.:	250 °C
Oven
Oven Temp.:	150 °C (hold 1 min) to 280 °C at 28 °C/min
Carrier Gas	He, constant flow
Flow Rate:	1.4 mL/min
Linear Velocity:	45.023 cm/sec @ 150 °C
Dead Time:	1.115 min @ 150 °C

Detector

Mode:

Scan

Scan Program:

Group	Start Time (min)	Scan Range (amu)	Scan Rate (scans/sec)
1	1.5	50-750	7.5

Transfer Line Temp.:

280 °C

Analyzer Type:

Quadrupole

Source Type:

Extractor

Source Temp.:

280 °C

Quad Temp.:

150 °C

Electron Energy:

978 eV

Solvent Delay Time:

1.5 min

Tune Type:

PFTBA

Ionization Mode:

Instrument

Agilent 7890B GC & 5977A MSD

Notes

Approximately 1 of mg sugar was dissolved in 100 μL of 40 mg/mL ethylhydroxylaminehydrochloride (EtOx) and heated at 70°C for 30 min. Samples were cooled to room temperature for approximately 5 min. 120 μL of N-Methyl-bis(trifluoroacetamide) (MBTFA) was added to each sample and then heated at 70°C for 30 min. Samples were diluted 1:100 in ethyl acetate.

Download PDF