2
Experimental Details
Consumables
Part Number
Column:
TRACE TR-FAME GC column,
260M238P
100 m × 0.25 mm × 0.20 μm
Septum:
Thermo Scientific BTO, 17 mm
31303211
Liner:
Thermo Scientific™ Split FocusLiner™, 3 × 8 × 105 mm 45350031
Column ferrules:
100% graphite ferrules for Thermo Scientific™ 29053488
TRACE™ injector 0.1–0.25 mm i.d.
Column ferrules:
Graphite/Vespel
®
for transfer line 0.1–0.25 mm i.d.
29033496
Injection syringe:
10 μL fixed needle syringe for Thermo Scientific™
36500525
TriPlus™ Autosampler
Vials and closures:
Thermo Scientific™ Chromacol™ 9 mm screw 0.3 mL 03-FISV (A)
fixed insert amber Micro+ vials
Chromacol 9 mm screw caps with Silicone/PTFE
9-SC(B)-ST101
septa
Syringes:
Thermo Scientific™ National™ 30 mm GMF Syringe
F2500-20
filter membrane, 3.1 µm pore size
Thermo Scientific™ National™ Target™ 3 mL plastic
S7510-3
disposable syringes
Sample Handling Equipment
Part Number
Thermo Scientific™ Reacti-Therm™ III Heating/Stirring Module
TS-18823
Thermo Scientific™ Reacti-Vap™ III Evaporator
TS-18826
Thermo Scientific Reacti-Vap Block
TS-18814
Thermo Scientific™ Reacti-Vial™ Reaction Vials 10 mL
TS-13225
Chemicals and Reagents
Part Number
Fisher Scientific™ HPLC grade hexane
H/0403/15
Fisher Scientific HPLC grade water
W/0106/17
Fisher Scientific HPLC grade methanol
M/4056/17
Fisher Scientific HPLC grade potassium hydroxide
S/9220/PB08
Thermo Scientific 14% BF
3
-methanol esterification reagent
TS-49370
Sample Preparation
Butter, margarine, and palm oil were treated by two derivatization methods. In the first method, potassium hydroxide /
methanol was used to esterify the fat samples [1]. This was then compared to an acidic derivatization method involving
BF
3
-methanol [2].
Base esterification:
A 50 mg liquid fat sample was weighed into Reacti-Vial containing
a magnetic stirrer and 1 mL of hexane and 2 mL of 4 mol/L potassium
hydroxide / methanol were added. The Reacti-Vial was capped and
placed in the Reacti-Therm module for 30 minutes at 50 °C. The
mixture was cooled to room temperature and 1 mL of water was then
added. After phase separation, an aliquot of the organic layer was
transferred to a fixed insert GC vial.
Acid esterification:
A 50 mg liquid fat sample was weighed into a Reacti-Vial containing
a magnetic stirrer and 1 mL of hexane and 0.5 mL of Thermo Scientific
14% BF
3
-methanol was added. The Reacti-Vial was capped and
placed in the Reacti-Therm module for 30 minutes at 50 °C. The
mixture was cooled to room temperature and 1 mL of water was then
added. After phase separation, an aliquot of the organic layer was
transferred to a fixed insert GC vial.
