9. Consumables
Fisher Scientific
Part Number
9.1
GC column –
26098-1420
TraceGOLD TG-5MS 5% diphenyl
and 95% dimethyl polysiloxane
stationary phase, 30 m, 0.25 mm ID,
0.25 µm film thickness (Thermo
Fisher Scientific, Bellefonte, PA USA)
9.2
SPME fiber –
57341-U
coated with PDMS, d
f
100 µm
Supelco
Bellefonte, PA USA
9.3
Headspace vials – 20 mL flat
3205551
bottom, clear glass, beveled edge
9.4
PTFE – faced butyl rubber septa
3205532
for headspace vials – 20 mm,
septa Butyl/PTFE
9.5
Capping device – Manual Crimper C4020-100
for 20 mm Aluminum Crimp Seals
9.6
Pipette Finnpipette 100–1000 µL 3214535
9.7
Pipette Finnpipette 20–200 µL
3214534
9.8
Pipette Finnpipette 10–100 µL
3166472
9.9
Pipette Finnpipette 500–5000 µL 3166473
9.10
Pipette Finnpipette 1000–10000 µL 3214536
9.11
Pipette holder
3651211
9.12
Pipette tips 0.5–250 µL, 500/box 3270399
9.13
Pipette tips 1–5 mL, 75/box
3270420
9.14
Pipette tips 100–1000 µL, 200/box 3270410
9.15
Pipette tips 20000–10000 µL,
3270425
40/box
9.16
Pipette Pasteur – soda lime
FB50251
glass 150 mm
9.17
Pipette suction device
3120891
9.18
Spatula, 18/10 steel
3458179F
9.19
Spatula, nylon
3047217
9.20
Wash bottle, PTFE
3149330
Glassware
9.21
Beaker, 50 mL
965 32 10
9.22
Beaker, 100 mL
965 32 20
9.23
Volumetric flask, 10 mL
FB50143
9.24
Volumetric flask, 25 mL
FB50147
10. Procedure
Preparation of the Instrument –
Before starting to work
with the instrument or preparation it for work in SPME
mode, please read carefully the relevant chapter of the
Thermo Scientific TriPlus Operating Manual and Section IV
in the Thermo Scientific TriPlus Standard Operating
Procedures. There is described all necessary maintenance
during installation of the SPME holder and SPME fiber.
10.1 Sample Preparation
Solid and Semi-solid matrices
10.1.1
Homogenize 150 g of sample in a high-speed
blender (soups, sauces and pesto) or in a Waring
laboratory blender (solid matrices like muesli) for
5 min, and then accurately weigh 0.1 g directly
into a headspace vial.
10.1.2
Add 10 µL of working standard solution of
dicyclohexylmethanol, 10 µL of standard solution
of coumarin-d
4
, and add 9980 µL of water using
micropipettes of appropriate sizes.
Liquid Matrix
10.1.3
Weigh 0.1 g directly into a headspace vial add
10 µL of working standard solution of dicyclo-
hexylmethanol, 10 µL of standard solution of
coumarin-d
4
and add 9980 µL of water using
micropipettes of appropriate sizes.
10.1.4
In both cases, add 2.5 g NaCl, seal with a
PTFE-faced butyl rubber septum and cap the
sample with the crimping device.
10.1.5
For calibration purposes, use blank foodstuffs
representative of each of the respective matrix types.
•
Liquid matrix (mainly representing alcoholic
drinks) comprising a 40% solution of aqueous
ethanol used as blank material
•
Semi-solid matrix (mainly representing sauces
and pesto) comprising pure tomato sauce used
as blank material
•
Solid matrix (mainly representing muesli)
comprising oat flakes used as blank material
For solid and semi-solid matrices, use the volumes of
standards and internal standards as shown in Table 1,
and for liquid matrices use corresponding volumes as
shown in Table 2.
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