5.2 Injection Standard
5-methylchrysene – 5-MChr (Dr. Ehrenstorfer)
5.3 Internal Standards
Anthracene-D10 – Ant-D10 (Sigma)
Benzo[a]pyrene-D12 – B(a)P-D12 (Sigma)
Benzo[ghi]perylene-D12 – B(g,h,i)P-D12 (LGC Standards)
Chrysene-D12 – Chr-D12 (Sigma)
5.4 Quality Control Materials
Petroleum Crude oil (NIST Standard Reference
Material
®
, 1582)
Aliphatic Hydrocarbons in 2,2,4-Trimethylpentane
(NIST Standard Reference Material, 1494)
6. Standards and Reagent Preparation
6.1
Stock solutions of 2 µg/mL of PAH standards
in toluene
6.2
Internal PAHs standard (IS) concentration:
2 µg/mL (Benzo[ghi]perylene-d
12
, Anthracene-d
10
,
Chrysene-d
12
) in toluene and 200 µg/mL
Benzo[a]pyrene-d
12
in cyclohexane
6.3
Working standard solution mixture of 16 PAHs
in toluene (100 ng/mL)
6.4
Working internal standard mixture of IS PAHs
in toluene (200 ng/mL)
6.5
Syringe standard, 5-methyl-chrysene (200 ng/mL)
in toluene.
6.6
Spiked solution of Petroleum crude oil (NIST 1582):
100 mg/mL in cyclohexane
7. Apparatus
Fisher Scientific USA
Part Number
7.1
Centrifuge, Heraeus
™
75-004-500
Multifuge
™
X3
7.2
Thermo Scientific 16 port SPE
03-251-252
vacuum manifold
7.3
Evaporator EVTM-130-32-16
3106395
(Fisher Scientific Germany)
7.4
Fisher precision balance
01918306
7.5
Vacuum pump
05-402-100
7.6
Rotavapor
®
R-210
05-024-21
7.7
Sartorius analytical balance
01-910-3224
7.8
Thermo sci. Barnstead
0905050
EASYpure
™
II water
7.9
Ultrasonic bath Elmsonic S40H 154606Q
7.10
ULTRA-TURRAX
®
–
1425980
dispergation tool
7.11
ULTRA-TURRAX –
14259023
Plug-in coupling
7.12
ULTRA-TURRAX
142259301
7.13
Vortex shaker
14505141
7.14
Vortex standard cap
14-505-140
7.15
GC column TR-50MS 30 m,
260R142P
0.25 mm ID, 0.25 µm film
7.16
TSQ Quantum XLS
™
Triple Quadrupole
Mass Spectrometer
8. Consumables
Part Number
8.1
GC vials
03393F
8.2
Pipette Finnpipette 100-1000 µL 14386320
8.3
Pipette Finnpipette 10-100 µL
14386318
8.4
Pipette Finnpipette 500-5000 µL 14386321
8.5
Pipette holder
14245160
8.6
Pipette Pasteur soda lime
136786A
glass 150 mm
8.7
Pipette suction device
03-692-350
8.8
Pipette tips 0.5 – 250 µL, 500/box
21377144
8.9
Pipette tips 1 – 5 mL, 75/box
2137750
8.10
Pipette tips 100 – 1000 µL,
2137746
200/box
8.11
Spatula, 18/10 steel
14356C
8.12
Spatula, nylon
NC9319088
8.13
SPE Hypersep SI,
03251270
200 mg/3 mL, 50 pc.
8.14
Tube holder
03840233
8.15
Wash bottle, PTFE
0340911A
Glassware
8.16
Beaker, 50 mL
FB10050
8.17
Fisherbrand test tubes
14-958D
8.18
Funnel, 55 mm
14353D
8.19
Glass tubes
14957E
8.20
Pasteur pipette
136786A
8.21
Round flask 50 mL, NS 29/32
9011835
(Fisher Scientific Germany)
8.22
Volumetric flask, 10 mL
FB40110
8.23
Volumetric flask, 25 mL
10200A
9. Procedure
9.1 Sample Preparation
Rinse the glassware with acetone before proceeding with the
method to avoid cross contamination. Homogenize a suitable
amount (e.g. 250 g) of oyster meat appropriately to give a
slurry using a high speed blender, e.g. ULTRA-TURRAX.
9.2 Extraction
9.2.1
Accurately weigh the homogenized sample
(ca. 2 g) into a glass tube.
9.2.2
Add 50 µL of PAH internal standard solution
to the sample.
9.2.3
Vortex the mixture for 10 s and wait 10 min for
equilibration.
9.2.4
Add 5 mL of hexane to the sample and put it into
an ultrasonic bath for 10 min.
9.2.5
Transfer the supernatant hexane layer into a 50 mL
round flask with a Pasteur pipette.
9.2.6
Repeat the extraction (9.2.4 and 9.2.5) three
more times.
9.2.7
Centrifuge for 5 min at 4500 rpm and 5 °C
and decant supernatant.
9.2.8
Evaporate to 1 mL under vacuum (220 mbar/50 °C).
